TW213901B - - Google Patents

Description

A6 B6 printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of the invention (1) Background of the invention The present invention has novel substituted hexahydroazazepines and tetrahydrobenzoazazepines containing such compounds. Pharmaceutical compositions and the use of such compositions in the treatment and prevention of central nervous system and intestinal disorders. The pharmaceutically active compound of the present invention is a selective CCK-B receptor antagonist. Cholecystokinin (CCK) is a 3-amino acid found and identified in 1971. (See Mutt e_t_ a 1.. Bioche ·. J., 125, 57 (1971)). It binds to its two receptors to carry out a biological response: 0 (: _ _ eight and (: (: 1 ^ one 8. (: (: 1 < one eight receptors are mainly located in the sac and pancreas, and CCK-induced enzyme secretion and gallbladder contraction during feeding. CCK-B receptors are located in the stomach, which involves acid secretion, and in the brain, it mediates pain and anxiety reactions. Several types are known to be used in these two subjects The body's potent and selective non-peptide antagonist (see MG Bock & Drugs of the Future, 16 (7), 631-640 (1991) and R. M. Freidinger, Med.

Res. Re v., 9.271-290 (1989)) ○ Merc-k ’s L-364, 718 (devazepide) is a selective CCK-A antagonist. (See O'Neill e_t_ a 1., Brain Res., 5 4 3. 287 — 290 (1990)). However, this compound proved to be clinically unavailable. Merck ’s beuzodiazepine L-365, 260 was found to be a selective CCK-B antagonist with analgesic effects on squirrel monkeys. (See O'Neill a_L-, Brain Res., 5 4 3, 287-290 (1990)) 〇Clarke-Da-vis · Cj? _ 9 8 8 was found to be induced by reversing the five stomach hormones in mice (please first Please pay attention to the page before filling out this page) i Pack · Order _ This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 g *) -4-2,13901

Charge, year vV A6 B6 V. Description of the invention (2) A selective CCK-B antagonist for the effect of anxiety response. (See Sj-Q-gh, et. Aj_., Proc. NatM. Acad. Sci .. US. 8 8 »1130-33 (1991)) 〇 General Summary of the Invention The compound of the present invention is related to the following formula (please read the back (Notes will be written on this page)

Η I1 or _install · order ·

The Ministry of Economic Affairs, Central Standards Bureau, Xinggong Consumer Cooperatives Co., Ltd. takes the following formula: Υ1 and Υ2 are each selected from phenyl, phenyl, pyridyl, furfuryl, pyrimidinyl, (C3-C8) linear or branched And (c5-c8) cycloalkyl groups, wherein the phenyl group, oxanyl group, pyridinium group, furyl group and pyrimidinyl group can be freely selected from one or two each selected from halo groups (such as 'gas group' atmosphere group , Bromo or bowl-based) '(Ci-Ce) burning group' (Ci-Ce) substituted by oxy, nitro, amine and trifluoromethyl substituents' and the ring paper size is applicable to China Gujia Standard (CNS) Grade A 4 (210 X 297 mm) A6

The alkyl group can be optionally substituted by one or two substituents each selected from (Cl-c6) alkyl groups: Z1 and Z2 printed by the Consumer Labor Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs are selected from halogen-containing groups, (Ci-c6 ) Alkyl, (Ci-Ce) thioalkyl '(Ci-Ce) alkoxy, trioxymethyl, (Cl-C6) alkoxycarbonylamino and nitro groups: R1 is phenyl, C 〇 2R2, S 〇2N R3R6 or C ON R4R5, wherein the phenyl group can be freely selected from one or two each selected from a halo group, (Ci-C6) halo group, (Cl-C6) halooxy group, nitro group, amine group And the substituents of the trimethyl group, and R2 »R 3 * R 4, RS and R6 are each selected from hydrogen, (C3-C12) alkyl and fused, saturated bi- or tricyclic carbon Ring system: W is hydrogen, chlorine or methyl. The invention also relates to pharmaceutically acceptable acid addition salts of compounds of formulae I and II. The acid used to prepare the pharmaceutically acceptable acid addition salt of the above base compound of the present invention is one that forms a non-toxic acid addition salt, that is, a salt containing a pharmaceutically acceptable anion, such as hydrochloric acid, hydrobromic acid, hydroiodide Acid, nitric acid, sulfuric acid, hydrogen sulfate, phosphoric acid, acid phosphoric acid, acetic acid, lactic acid, citric acid, acid citric acid, tartaric acid, hydrogen tartrate, succinic acid, maleic acid, fumaric acid, gluconic acid, hemp sugar Acid, benzoic acid, methanesulfonic acid, ethanesulfonic acid, benzenesulfonic acid, p-toluenesulfonic acid and pamoate (ie, 1, 1'-extended methyl-bis- (2-hydroxy-3-- Acid salt)]. As used herein, alkyl, unless otherwise stated, includes a linear, branched or cyclic moiety or a combination of saturated monovalent hydrocarbon groups ° As used herein, halo ', unless otherwise stated, includes chloro 'Fluoro, bromo and iodo. (--- install ------ ΤΓ ------ marry (to read the notes on the back first and then this page) This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -6 A6 B6 printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of the invention (4) The preferred compounds of the present invention are compounds of formula I, where both γ2 and γ2 are phenyl, or γ / and γ One of 2 is oxhexyl. Other preferred compounds of the invention are compounds of formula I, where γ2 is phenyl. Preferred compounds of the invention include the following: 2 — [3 — (3 — (3-thiomethyl Phenyl) ureido)-2-oxo-5-benzyl-2, 3, 4, 5-four gas-1 H-(1) Benzo Krypton leather-1-yl] tert-butyl acetate; 3 — ((3-Gasophenyl) adenyl) -7-hexyl-1 (Ν—t-butoxycarbonylmethyl) hexahydroazazepine-2-one; 3 1-((3-tolyl) gland Group) a 7-cyclohexyl one (N_t-butoxycarbonylmethyl) hexahydroazepine 2-ketone; 3-((3_ gas phenyl) ureido)-7-cyclohexyl one (N -1 adamantane gas carbonylmethyl) hexahydrogen Aza leather-2-ketone; 3-((3-gasphenyl) ureido) -7-cyclohexyl-1- (N-2-adamantane gas carbonylmethyl) hexahydroazazepine-2-one; 3 — ((3-tolyl) ureido) —7—cyclohexyl— (N-1—adamantyloxycarbonylmethyl) hexahydroazazepine—2__; 3 — ((3-tolyl) adenyl) -1 7-Cyclohexyl one (N 2 -adamantane gas carbonylmethyl) hexahydroazazepine 2 -one;

3_ ((3 -methylphenyl) adenyl) -7-cyclohexyl_ (N-t-butoxycarbonylmethyl) hexahydroazazepine-2-one;

3 — ((3-methylphenyl) ureido) —7 —cyclohexyl mono (N _1 adamantane gas carbonylmethyl) hexahydro radon complex leather 2-one ketone; this paper is applicable to the Chinese HJ standard (CNS ) A 4 specifications (210 X 297 public goods) ~~ _ ~~ I-_ ---------------- J ------ install ------ order (Please read the note $ item on the back and then fill out this page) A6 B6 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Invention Instructions (5) 3 — ((3-Methoxyphenyl) ureido) 1 7 — Cyclohexyl one (N 2 -adamantyloxycarbonylmethyl) hexahydroazazepine 2 -one; 3-((3-gas phenyl) ureido) 5,7 -diphenyl one (Ν— t-butoxycarbonylmethyl) hexahydroazepine-2-ketone; 3-((3-tolyl) ureido) -5,7-diphenyl- (N-t-butoxycarbonylmethyl) Hexahydroazazepine-2-ketone; 3-((3-methoxyphenyl) ureido) -5,7-diphenyl- (N-t-butoxycarbonylmethyl) hexahydroazaza-1 2-keto; 3-((3-chlorophenyl) ureido) -5,7-diphenyl- (N-1-adamantyloxycarbonylmethyl) hexahydroazaaza-2 — Ketone; N — third butyl 2 — [3 — (3 — (3-phenyl) gland) — 2 — gas — 5 —phenyl — 2, 3, 4, 5 — tetrahydro-1H- ( 1) Benzoazepine-1-yl] acetamide acetate; N-third butyl 2- [3- (3- (3-tolyl) adenyl) -2-oxo-5-phenyl-2- , 3, 4, 5 — tetrahydro- 1H _ (1) benzoazepine-1 1-yl] acetamide acetate; N- tertiary butyl 2-[3-(3-(3-methane phenyl ) Adenyl) -2-oxo-5-phenyl-2, 3, 4, 5-tetrahydro-1H_ (1) benzodiazepine-1 yl] acetamide acetate; N — third butyl 2 — [3 — (3 — (3-thiomethylphenyl) adenyl) -2—gas-5—phenyl-2, 3, 4, 5_tetrahydro-1H_ (1) benzodiazepine-1 1-yl] acetamide acetate; N, N — bis (ethylene-propyl) 2- [3- (3- (3-gasphenyl) adenyl)-2-gas-5-phenyl-2, 3, 4, 5—4 (please read the precautions on the back and then fill out this page). Installed. Order _ This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -8-139〇i A6 B6 Printed by the Employees ’Cooperative of the Central Bureau of Standards of the Ministry V. Description of the invention (6) Hydrogen-1H— (1) Benzoazepine-1-yl] acetamide acetate; N, N—di (2-propyl) 2— [3-(3-(3-tolyl) ureido)-2-gas-5-phenyl-2, 3, 4, 5-tetrahydro-1H-(1) benzodiazepine-1-1 〕 Acetamide; N, N — bis (2-propyl) 2 — [3 — (3 — (3 — methylphenyl) ureido) — 2 — gas 5 — phenyl 2, 3, 4 , 5 — tetrahydro-1H— (1) benzoazepine-1-yl] acetamide acetate; N, N — bis (2-propyl) 2 — [3 — (3 — (3 -thiomethyl Phenyl) urea) 2-gas-1 5-phenyl-2, 3, 4, 5 tetrahydro-1H-1 (1) benzoazepine-1 1-yl] acetaldehyde acetamide; 2- [3 — (3 — (3-gasphenyl) ureido) —2-oxo-5-phenyl—2, 3,4, 5-tetrahydro-1H — (1) benzodiazepine-1 1-yl] Third butyl acetate; third butyl 2- [3- (3- (3-tolyl) ureido) one 2-gas one 5-phenyl one 2, 3, 4, 5-tetrahydro one 1H- (1) Benzene Azazepine-1 1-yl] tert-butyl acetate; 2- [3- (3- (3-methylphenyl) ureido)-2-gas-5-phenyl-2, 3, 4, 5-tetrahydro-1H- (1) benzoazepine-1-yl] N-tert-butyl acetate; N-tert-butyl 2- [2-oxo-3-((3-tolyl) Ureido)-5,7-diphenylhexahydroazazepine-1-yl] acetamide; N-third butyl 2- [2-gas-3-((3-triphenyl) urea Base) a 5, 7_ diphenyl hexahydroazazepine a 1-yl] Acetyl Acetate (please read the precautions on the back before filling the nest page). 丨 installed. Ordered. This paper size is applicable to Chinese national standards ( CNS) A4 specifications (210 X 297 mm) -9-Α6 ____ Β6 V. Description of the invention (7) Amine; Ν—Second butyl 2— [2-—gas 3 — ((3-methyl gas phenyl) Dolphinyl) a 5,7-diphenyl hexahydroazepine leather a 1-yl] aldamine acetate; printed by the Ministry of Economic Affairs Central Standards and Consumers Cooperatives N- third butyl 2-C phenyl) urea ) One 5 * 7 Alacetal acetamide 9 N-Third Group 2-C thiophenyl) m group) 5% 7 Acetamide Acetate 1 N-third butyl 2-C) urea) 5 5, 7 Diphenylamide • $ Ν-Third Butyl Group 2 -C aminophenyl) m group) — 5 > 7] Aldamine acetate 9 N-third butyl 2 1 C) urea group) 5 9 7 — diphenylamine •% Ν _ third Butyl 2-C group) 5-Phenyl-8-Methyl 1 Η-(1) Benzene leather N- the third butyl 2-C) 5-Phenyl-9-methyl The size of this paper is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) 2 —Gas 3 — ((3 —Trifluoromethyldiphenyl hexahydroazaza-1 leather) 2—Gas generation A 3- ((3-Methyl-diphenyl hexahydro-aza-leather leather 1 1-yl 2-gas- 3-((3-gas phenyl- hexahydro-aza-leather leather 1- 1-yl] acetic acid 2-gas ~ 3 — ((3-Dimethyl-diphenyl hexahydroazaza leather 1-one 2-oxo 3- — ((3-ethylphenyl hexahydroazaza leather 1-one] ethyl Aldehyde 2 —gas》 3 — ((3-tolylurea-2, 3, 4, 5-tetrazol-1-yl) acetamide acetate; 2-oxygen ~ 3- (3-tolyladenyl 2, 3,4 , 5-Tetrahydro-1H, printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 2139G1 a6 _B6 V. Description of the invention (8) One (1) benzodiazepine leather 1-amino] acetamide acetate; N — third butyl Base 2_ [2-gas-1-3- (3-tolylurea) -5-phenyl-1-7-tri-2,3,4,5-tetrahydro-1H-1 (1) benzodiazepine-1-1 Group] Acetaldehyde aldehyde amine; 2 — [2- Oxygen 3-(3- Toluo waist group)-5-(4- Fluorophenyl)-2, 3, 4, 5-tetrahydro_1H- (1) benzene Bacteria leather -1-yl] N- third butyl acetate; N- tertiary butyl 2-[2-gas 3-(3-tolylurea)-5-(4- gas phenyl)- 2, 3, 4, 5 -tetrahydro-1H- (1) benzoazepine-1-yl] acetamide acetate; N — third butyl 2- [2-gas-3-(3-toluene Base)-5-(4-tolyl)-2, 3, 4, 5-tetrahydro-1H-(1) benzoazepine-1-yl] acetamide; N-third Base 2-[2-Gas 3-(3-Toluenyl)-5- (2-fluorophenyl)-2, 3, 4, 5-tetrahydro-1H One (1) benzodiazepine_ 1 monoyl] aldamine acetate; N — third butyl 2 — [2 — gas 3 — (3-tolylurea) — 5 — (3 — gas phenyl) — 2, 3, 4, 5 — four Hydrogen- 1H- (1) benzoazepine-1-yl] acetaldehyde acetamide; N — third butyl 2 — [2 —gas 3 — (3-tolylurea) -5- (3,4 (Dichlorophenyl) -2, 3, 4, 5 — tetrahydro-1H — (1) benzoazepine-1-yl] acetamide acetate; N — (1,1 dimethyl) propyl ) One 2-[2-Gas One 3 One ((3-Tolyl) Urea) One 5-Phenyl One 2, 3, 4, 5 (Please read the precautions on the back before filling this page) Applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -11-A6 2i39Gi _____B6_ V. Description of the invention (9) tetrahydro-1H_ (1) benzodiazepine 1yl] acetaldehyde acetamide; (N-(1-methyl) cyclohexyl)-2_ [2 monooxygen ((3-tolyl) ureido)-5-phenyl-2, 3, 4, 5-tetrahydro-1H_ (1) benzoazepine-1-yl] acetaldehyde; N-third butyl 2- [2-gas-3- (3-tolyl) -5- Cyclohexyl-2, 3, 4, 5 — tetrakis-1H — (1) benzodiazepine-1 1-yl] acetamide acetate; examples of other compounds of the present invention include: N — third butyl 2 — [ 2-gas-3-((3-tolyl) ureido) -5-phenyl, 7- (3-pyridyl) hexahexaazazepine-1-yl] acetaldehyde acetamide; N—third butyl Yl 2- [2-oxo-3-((3-tolyl) adenyl) -5-phenyl, 7- (2-pyridyl) hexahexahydrogen-l-yl] acetamide acetate; N —Third butyl 2- [2-gas-3-((3-tolyl) ureido) -5-phenyl, 7- (4-pyridyl) hexahydroazazepine-1-yl] acetic acid Acetamide; N — third butyl 2 — [2 — gas 3 — ((3-tolyl) ureido) 5 — phenyl, 7 — (3 — sleeping and drinking) 1 hexahydroazapyridine 1 1 monoyl] acetamide acetate; N — tertiary butyl 2- [2-gas-3-((3-tolyl) ureido) -5 Phenyl, 7- (2_sleep drinking base) hexahydroazaza leather 1- 1] aldamine acetate; (please read the note mF on the back before filling in this page)-Pack. Order-Central Bureau of Standards, Ministry of Economic Affairs Printed by Beigong Consumer Cooperation Co., Ltd. The paper size is in accordance with Chinese National Standard (CNS) A4 (210 X 297 mm) -12-213901 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (10) N-tert-butyl 2- [2-gas-3-((3-tolyl) adenyl) -5-phenyl, 7- (2-pyrimidinyl) hexahydroazazepine-1-yl] Acetamide; N — third butyl 2- [2-oxo-3-((3-tolyl) ureido) -5-phenyl, 7- (4-pyrimidinyl) -hexahydroaza- 1 monoyl] acetamide acetate; N-third butyl 2- [2-oxo 3-((3-tolyl) adenyl) -5- (3-gasphenyl), 7-phenylhexa Hydrazine leather 1- 1] Acetamide Acetate; N — third butyl 2- [2-gas- 3-((3-tolyl) ureido)-5- (4-gas phenyl), 7- Phenylhexahydroazazepine-1-yl] acetamide acetate; N —Third butyl 2- [2-oxo-3-((3-tolyl) ureido) —5- (3-chlorophenyl), 7-phenyl-hexahydrogenated leather -1-yl] acetic acid Acetylamine; N-tert-butyl 2- [2-gas-3-((3-tolyl) ureido) -5- (3-trifluoromethylphenyl), 7-phenyl-hexahydronitrogen Miscellaneous leather 1- 1] Acetamide; N- third butyl 2- [2-oxo 3- ((3-tolyl) ureido)-5- (3-tolyl), 7-phenyl Hexahydroazazepine-1-yl] acetamide acetate; N-third butyl 2- [2-gas-3-((3-tolyl) ureido) -5- (4-tolyl), 7-Phenylhexahydror Krypton leather-1 1-yl] Acetamide; This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 public *) _ 13 _ (Please read the notes on the back first Re-write this page)-installed. Ordered--I-quan · Printed by the Ministry of Economic Affairs Central Standards Employee Consumer Cooperatives A6 B6 V. Description of the invention (11) N—Third Butyl 2— [2—Gas 3— ( (3-tolyl) adenyl) 5- (4-methylphenyl), 7-phenyl-6 Gas-leather-1 yl] acetamide acetate; Ν—third butyl 2- [2-gas-3-((3-tolyl) ureido) -5- (3-methylphenyl), 7 —Phenylhexahydroazazepine-1-yl] acetaldehyde acetamide; Ν—third butyl 2_ [2-gas-2- (3- (tolyl) ureido) -5- (3-pyridyl ) · 7-Phenylhexahydroazazepine-1-yl] acetaldehyde acetamide; Ν—third butyl 2- [2-oxo-3-((3-tolyl) ureido) -5- ( 3-Pinyl), 7-phenyl-hexahydroazazepine-1-yl] acetamide acetate; N-third butyl 2- [2-oxo-3-((3_tolyl) ureido ) A 5-(4 a sleeping sulfanyl), 7-phenyl-hexahydroazazepine -1-yl] acetamide acetate; N-third butyl 2_ [2- gas 1 3-((3-tolyl ) Ureido) 5- (2-pyridyl), 7-phenyl-hexahexaazazepine-1-yl] acetaldehyde acetamide; N — third butyl 2 — [2- —gas 3 — (( 3-tolyl) ureido) -5-cyclohexyl, 7-phenyl-hexahydroazazepine-1 1-yl] acetyl acetate ; N — (1, 1-dimethyl) propyl) 2 — [2-gas 3 ~> ((3-tolyl) adenyl)-5, * 7-one phenyl six gas Leather 1 1 base] Acetamide; (Please fill in the precautions on the wf side first, then fill in this buy> 丨 Packing. Ordered · This paper size is suitable for China National Standard (CNS) A 4 specifications (210 X 297 mm) -14-A62139G1 Fifth, the description of the invention (12) N — (1, 1 dimethyl) benzyl) 2 one [2-oxygen one 3-((3-tolyl) knee group) one 5, 7 one two Phenyl-hexahelium aza-leather-1 yl] acetaminophen; N — (1-methyl) oxhexyl) 2 — [2- gas 1 3-((3 -tolyl) urea)-5. 7-diphenyl-hexahydroazatrile] acetamide acetate; N — (1 monomethyl) pentyl) 2 — [2 — gas 3 — ((3-tolyl) ureido) 1 5, 7-diphenylhexahydroazazepine-1-yl] acetaldehyde acetamide; N-third butyl 2- [2-gas-3-((3-methylaminophenyl) ureido) A 5,7-diphenylhexahydroazazepine-1-yl] acetamide acetate; N — third butyl 2 — [ 2-Gas 3- ((3-methyl, N-acetaldehyde) adenyl)-5-cyclohexyl, 7-phenyl-hexahydrogen leather-1-yl] acetamide; N- third butyl Yl 2- [2-gas-3- (3- (N-methyl, N-methanesulfonaldehyde) ureido) -5-cyclohexyl, 7-phenyl-hexahydroazazepine-1-yl] acetic acid Amine; N — tert-butyl 2-[2 -gas one 3-((3-two please read the note on the back and then this page). Binding. Order-Central Economic Bureau of the Ministry of Economy ®: Industrial and Consumer Cooperative Printed phenyl) ureido) _5, 7-diphenyl hexahydroazazepine one] aldamine acetate; ethylamine N — third butyl 2_ [2_Gas 3 — ((3 — iso Propylaminophenyl) urea) 5,7—] Aldylacetate; Hexaarginine leather-Basic paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm)

V. Description of the invention (13) Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs N-third butyl 2- [2-gas-1 3-((q 1 ~ butylaminophenyl) ureido) -5, 7-diphenyl-hexahydroazazepine-i-yl] acetamide acetate; N-second butyl 2- [2-gas-2-((3-isopropylphenyl) adenyl) -5, 7-diphenylhexahydrogen-l-yl] acetamide acetate; N-second butyl 2-mono [2-monofluoro-3-((3-butylphenyl) ureido) -5,7 ~ Diphenylhexahydroazazepine-1-yl] acetaldehyde acetamide; (N — (1,1-dimethyl) phenyl) 2 — [2- —gas 3 — ((3 — 甲 本Radical) adenyl) 5-phenyl-2, 3, 4, 5-tetrahydro-1 Η- (1) benzodiazepine-1 yl] acetaldehyde acetamide; (Ν— (1 monomethyl ) Cyclopentyl) a 2- [2-oxo 3_ ((3-tolyl) adenyl) a 5-phenyl one 2, 3, 4, 5-tetrahydro-1H_ (1) benzodiazepine leather A 1-one] acetamidase; Ν—third butyl 2- [2-oxo 3 -— ((3-dimethylaminophenyl) ureido) —5-phenyl- 2, 3,4,5-tetrahydro-1H— (1) benzoazepine-1-yl] acetamide; Ν —third butyl 2 — [2 ~ gas-1 3 (((3- (Aminophenyl) ureido) 5-phenyl-2,3,4,5-tetrahydro-1H- (1) benzoazepine-1 1-yl] acetamide acetate; Ν—third butyl 2 — [2 —Gas 3 — ((3 — (Ν — methyl, Ν —acetyl) adenyl) -5—phenyl-2, 3, 4, 5 — tetrahydro-1H_ (1) benzo Azapyridine-1-yl] aldamine acetate; the paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 ¾%) ~ ---------------- ^ ------- Dressing ------ Ordering ----- Quan (please read the precautions on the back before filling in the clothing page). External _B6_ V. Description of Invention (14) N — Third Butyl 2 — [2 —Gas 3-((3- (N-Methyl, N-Methanesulfonyl)) ureido) -5-Phenyl-2, 3, 4, 5-Tetrahydro-1 H — (1) benzodiazepine-1-1-yl] acetaldehyde acetamide; Ν—third butyl 2- [2-gas-1-3-((3-diethlylphenyl) ureido) -5 Phenyl one 2, 3, 4, 5 — four gas one 1Η — (1) benzene Azazepine-1-yl] acetaldehyde acetamide; Ν—third butyl 2- [2-gas-3-((3-isopropylaminophenyl) adenyl) -5-phenyl-2, 3 , 4, 5-tetrahydro-1H — (1) benzoazepine-1-yl] acetaldehyde acetamide; Ν —third butyl 2 — [2- —gas 3 — ((3 — t-butylamine Phenyl) ureido) 5-phenyl-2, 3, 4, 5-tetrahydro-1H- (1) benzoazepine-1 1-yl] acetamide acetate; N-third butyl 2 — [2—Gas 3 — ((3 —Isopropylphenyl) ureido) 5—Phenyl 2, 3, 4, 5 — Tetrahydro-1H 1 (1) Benzoaza-1 Monoyl] acetamide acetate; N-third butyl 2- [2-gas-3-((3-septabutylphenyl) ureido) -5-phenyl-2, 3, 4, 5- Tetrahydro-1H_ (1) benzodiazepine-1 1-yl] acetamide acetate; N — third butyl 2 — [2-oxo 3 — (3-tolylurea Ministry of Economic Affairs Central Standards Bureau employee consumer cooperative Printed (please read the precautions on the back before filling in this page). Installed-• Dai. Base)-5-phenyl-8-methoxy-2, 3, 4, 5-tetrahydro 1H — (1) benzodiazepine-1 1-yl] acetamide acetate; N — third butyl 2 — [2 — gas 3 — (3-tolylureido) 5—phenyl 8— Ethoxy-2, 3,4, 5_tetrahydro-1H — (1) benzodiazepine-1 1-yl] acetamide acetate; this paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 Mm) -17-21 ^ 901 V. Description of the invention (15) N-Third butyl 2 ~ [2-yl) -5-phenyl-8 ~ Gas-1 (1) benzodiazepine leather-N- Third butyl A6 B6 2 group] Aldehyde acetamide; 2 'C 2 group) 5-Phenyl 8-gas-one (1) benzoazepine-i N-T-butyl group) 5- Phenyl-7- · methoxy 1H— (1) benzodiazepine_

One gas one 3-(3-tolyl gland, 3, 4, 5-tetrahydro one 1H

One gas one 3-(3-tolyl gland, 3, 4 »5-tetrahydro one 1H -2 -yl] aldamine acetate; [2 (please read the note on page f and then f page) Oxygen 3- (3-tolylurea 2, 3, 4, 5-monoyl] acetamide acetate; tetrahydro-N-third butyl group) 5-phenyl-7-gas-one (1) benzoazepine leather —1 N -third butyl 2-gas-3- (3-tolylurea 2, 3,4,5-tetramethyl-1H group) aldamine acetate; 2 ~ [2 groups) _5-phenyl-7 —Trifluoromethyl-1H— (1) benzoazepine ~ Ν—third butyl 2- [2-monooxa 3_ (3-monotolylurea-oxa 3- (3-yl-2,3, 4, 1 mono] Aldamine acetate tolyl gland 5-tetrahydro-binding. Thread.) 5-phenyl-8-trifluoromethyl ~~ 2,3,4,5 — tetrafluoro 1 1- Base] Acetaldehyde aldehyde amine; Printed by the Ministry of Economic Affairs Central Standard Employee Consumer Agency—1H— (1) Benzazepine ~ N—Second Butyl 2— [2-Gas 3- (3-Tolylurea ) A 5-(3 -fluorophenyl) ~ 1 Η-(1) benzodiazepine-1 Ν_third butyl 2- [2-yl] _5— (3-trifluoromethyl phenyl hydrogen A 1Η— (1) benzoazepine 2,3, 4,5-tetra-fi-mono] acetamide acetate; a gas _3 -— (3-yl) -2,3,4--1 1-yl] acetic acid Acryloyl Gland, 5-Tetraamine; This paper scale is applicable to the specifications of the middle-sleepy country Liang Zhun (CNS) A 4 (210 X 2 Kuo Gong *) -18-A6 B6 Printed by the Employees Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy Description of the invention (16) N — Third butyl 2 — [2 — Gas 3 — (3-tolylureido) — 5 — (4- Trifluoromethylphenyl) — 2, 3, 4, 5 — Tetrahydro-1H— (1) benzocyano-leather-1-yl] acetamide acetate; N — tertiary butyl 2 — [2 —gas-1 3 — (3-tolyladenyl) —5— (3 —Dimethylaminophenyl) -2, 3,4, 5-tetrahydro-1H_ (1) benzoazepine-1 1-yl] acetamide acetate; N — third butyl 2 — [2- gas A 3- (3-tolyl ureido) a 5- (3-sulfonamide phenyl) a 2, 3, 4, 5-four gas _1H — (1) benzodiazepine leather a 1-yl] Acetamide; N—Third butyl 2- [2-Gas 3- (3-Tolylurea) -5— (3-—Acetylamido Phenyl) -2, 3, 4, 5 tetrahydro-1 H_ (l) benzodiazepine-1 1-yl] acetamide acetate; N — third butyl 2 — [2 — gas 3 — ( 3-tolyl ureido) 5- (3, 4-difluorophenyl) -2, 3, 4, 5-tetrahydro-1H_ (1) benzodiazepine-1 1-yl] acetamide acetate; N —Third butyl 2 — [2 —Gas 3 — (3-Tolylurea) —5— (3, 4-Xylyl) —2, 3, 4, 5—Tetrahydro-1H_ (1 ) Benzoazepine-1 yl] acetamide acetate; N — third butyl 2 — [2-oxo 3 — (3-ethylphenylureido) — 5 — (4-gasphenyl) 3, 4, 5 — four gas-one 1H — (1) benzoazepine-1-yl] acetaldehyde acetamide; N-(1, 1-xylyl) 2 — [2-gas one 3--(3 A tolyl ureido group) — 5 — (4 — argon phenyl) — 2, 3, 4, 5 — four gas — 1 Η — (1) benzodiazepine -1- mono] acetamide; (please Read the precautions on the back first and then fill out this page) This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -19-A6 B6 213901 V. Description of the invention (17 ) N —Third butyl 2 — [2 ~ oxo 3 — (3- dimethylaminophenylureido) 5 — (4 helium phenyl) — 2, 3, 4, 5 —tetrahydro_ 1H — (1) benzodiazepine-1 monoyl] acetaldehyde acetamide; N —third butyl 2 — [2-gas-1 3- (3-dimethylaminophenylureido) 5— ( 4 monomethylphenyl) -2, 3, 4, 5 — tetrahydro-1H — (1) benzodiazepine-1 monoyl] acetaldehyde acetamide; N — (1,1-dimethylpropyl ) 2-[2-gas 3_ (3-tolyl ureido)-5-(4- methylphenyl)-2, 3, 4, 5-tetrahydro-1H-(1) benzoazepine leather A 1-yl] acetamide acetate; N — third butyl 2- [2-gas- 3-(3-ethylphenyl adenyl)-5-(4-phenyl phenyl)-8-methyl one 2, 3,4, 5 -tetrahydro- 1 Η-(1) benzogas mixed leather-1 -yl] acetamide; N — (1,1 dimethylpropyl) 2 — [2 ~ gas A 3 — (3 —tolyl ureido) _ 5 — (4 -gas phenyl) 8 methyl 2, 3,4,5-tetrahydro one 1H — (1) benzodiazepine one 1 one Acetylacetate ; N- tertiary butyl 2- [2- gas-3- (3 ~ dimethylaminophenyl adenyl)-5- (4-gas phenyl)-9-methyl 2, 3, 4, 5 _Tetrahydro-1H — (1) benzodiazepine-1-yl] acetamide acetate; N-third butyl 2- [2-oxo_3-a (3-dimethylaminophenylureido) -5-(4-methylphenyl) ~ 8-gas-2 3, 4, 5-tetrahydro- 1H-(1) benzodiazepine 1] acetic acid This paper scale is applicable to the β national standard (CNS ) A 4 specifications (210 X 297 mm) ---------------- ^ ------- installed ------ ir ----- (please Read the notes on the back first and then fill out this page) Printed by the Male Workers' Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 20 0.1: ^ 901 A6 B6 V. Description of the invention (18) Aldimine; N — (1, 1 ~~ dimethyl Phenyl) 2- [2-oxo-3 ~ 3-tolyl ureido)-5- (4-monomethyl, 3,4, 5-tetra- radon-1H- (1-ylphenyl) -8- radon-2 ) Benzodiazepine monoyl] acetamide acetate; N-(1, 1 -dimethyl 3-ethylphenylureido)-5, 2, 3,4, 5-tetrahydromonoyl] acetaldehyde acetamide; Phenyl group) 2- [2-oxygen 3 ~ one (4 Methylphenyl)-8-gas 1 Η-(1) benzodiazepine "1 (please read the notes on the back before filling in this N-(1,1 dimethylphenyl) 2-[2- Oxygen 3-3-dimethylaminophenylureido)-5-gas-2, 3, 4, 5-tetrahydro-1H amine; (4-tolyl)-8-(1) benzodiazepine Miscellaneous leather 1-yl] Acetyl Acetate N — (1, 1-dimethylphenyl) 2 — [2-oxo ~ 3 3-dimethylaminophenylureido) 5 — (-2, 3, 4 , 5 — Tetrahydro- 1H — 4-Monophenyl) ~ Gas (1). Binding-Binding-Printed by the Ministry of Economic Affairs, Central Bureau of Industry and Commerce Employee Consumer Cooperatives, a base] Acetamide N- (1, 1-toluene ) _ 3, 4, 5 — Alkyl tetraacetate; Ν-(1, 3-ethylphenylurea 2,3,4,5 1_xylyl) 2_ [2- —Gas 3 5-(4 hydrogen A 1 Η (3 methyl phenyl)-8-methyl-2-benzoazepine-1 ~ yl] (1) 1_ dimethylpropyl) 2-[2-gas-3 yl)-5 -(4 -tetrazol-1 1 Η-chlorophenyl) -8-methyl g 1) benzoazepine leather ~ 1 This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) 21 A 6 B6 Printed by R Industrial and Consumer Cooperation, Central Bureau of Standards, Ministry of Economic Affairs. 5. Description of the invention (19) yl] acetamide acetate; N— (1,1 dimethylpropyl) 2- [2-oxo-3— ( 3-Dimethylaminophenylureido) 5- (4-monochlorophenyl) ~ 8-methyl-2,3,4,5-tetrahydro-1H— (1) benzodiazepine-1 Monoyl] acetaldehyde acetamide; N, N-di (third butyl) 2- [3- (3- (radon phenyl) ureido)-2-gas- 5-phenyl-2, 3, 4, 5-tetrahydro-1H— (1) benzoazepine-1-yl] acetaldehyde acetamide; N, N-di (third butyl) 2- [3- (3- (tolyl) ureido) 1-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H- (1) benzodiazepine-1-yl] acetamide acetate; N, N-di (third butyl ) 2-[3-(3-(methoxyphenyl) adenyl)-2-gas-5-phenyl-2, 3, 4, 5-tetrahydro-1H-(1) benzodiazepine leather 1-yl] acetamide acetate; 3- ((3-chlorophenyl) adenyl)-7_ (2, 6-dimethylcyclohexyl)-(N-t-butoxycarbonylmethyl)-hexahydro nitrogen Leather 2-ketone; 3-((3-tolyl) ureido) -7- (2,6-dimethylcyclohexyl)-(N-t-butoxycarbonylmethyl) -hexahydroazaza — 2-keto; 3 — ((3-methoxyphenyl) -7— (2,6-dimethylcyclohexyl) — (N—t-butane carbonylmethyl) —hexahydroazaaza-2 One ketone; 3-((3-methoxyphenyl) ureido) _5-phenyl-7-cyclohexyl- (N-1-1-adamantanecarbonylmethyl) -hexahydroazazepine-2-bream; (please Read the note on the back first, and then write this page} — Binding. Order-4 This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 common patchouli)

V. Description of the invention (2Q >

3 — ((3-methylphenyl) ureido) — 5-phenyl r cyclohexyl mono (N—2-adamantane carbonylmethyl) — hexahydroazepine ~ ketone; 3 — ((3- toluene Base) ureido) _5-phenyl》 7-bad hexyl _ (N_l_adamantane gas carbonylmethyl)-hexahydroazepine ~ ketone; 3-((3-tolyl) ureido)-5-benzene Base 7-cyclohexyl one (N 2 -adamantane gas carbonylmethyl) hexahydroazazepine ~ 2 __ ketone; 3 — ((3-cyanophenyl) ureido) 5_phenyl-7 »^^ Base one (N-1 -adamantyloxycarbonylmethyl) hexahydroazazepine ~ 2__ ketone; and 3-((3-aminophenyl) ureido)-5-phenylcyclohexyl one ( N — 2 —adamantane gas carbonylmethyl) hexahydroazazepine 2 — _〇 The present invention also relates to a compound of the following formula R · XY I < -please listen to the precautions before respecting the face; 8 ^ This page > Ί 丨 Installation and ordering, Λ-. Printed by the Central Standards Bureau of the Ministry of Economic Affairs, Wgong Consumer Cooperative

Where R7 is hydrogen or one of the bases defined by R1 above, R8 is a desert, an amine group or an azido group and Y1 is as defined above. Such compounds can be used as intermediates in the synthesis of compounds of formula Π. The standard of clothing paper is in accordance with Chinese family standards (CNS> A4 specifications (210 X 297 mm) -23 ~ ~ A6 Printed by the Central Standards Bureau of the Ministry of Economic Affairs, Industry and Consumer Cooperatives V. Description of invention (21) The invention also relates to a A pharmaceutical composition for the treatment or prevention of mammals, including humans, selected from conditions containing pain, intestinal disorders such as ulceration and colitis, and central nervous system disorders such as Giulu and fear disorders, which include treatment Or a compound of formula I or I effective in preventing such conditions, or a pharmaceutically acceptable salt thereof, and a pharmaceutically acceptable hip. The present invention also relates to a method for treating mammals, including humans, selected from Conditions that include pain, gastrointestinal disorders such as ulcers and colitis, and central nervous system disorders such as anxiety and fear conditions, which include administering to the mammal an effective amount of a compound of formula I or I, or a pharmaceutical thereof The present invention also relates to a pharmaceutical composition, which is used to antagonize the effectiveness of cystoclastin in mammals, including humans, which includes effective antagonists The amount of cystoconstrictin of the compound of formula I or I, or a pharmaceutically acceptable salt thereof, and a pharmaceutically acceptable carrier. The present invention also relates to a method of antagonizing the efficacy of cystotropin in mammals, including humans, It includes administering an effective amount of a compound of formula I or I, or a pharmaceutically acceptable salt thereof, to the mammals to antagonize the gallbladder hormone. The present invention also discloses a pharmaceutical composition for treating or preventing gallbladder contraction in mammals, including humans Barriers of interleukins, which include compounds of formula I or I, or a pharmaceutically acceptable salt thereof, and a pharmaceutically acceptable carrier in an amount effective to antagonize cholecystokinin, and a pharmaceutically acceptable carrier. The invention also relates to a method for treating or Prevention of cholecystokinin-mediated disorders in mammals, including humans, which includes the administration of an antagonistic amount of the compound of formula I or I to the mammal's membranous contractile hormone, or its pharmacologically acceptable (Fill in this page again) • 丨 Installation-Order · 丨 Kang · This paper standard is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 mm) -24-Industrial and Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs Preparation 5. Description of the invention (22) Accepted salt. The present invention also relates to a pharmaceutical composition for the treatment or prevention of mammals, including humans, with self-contained pain, intestinal obstructions such as ulcers and colitis, and the central nervous system Disorders, such as anxiety and fear conditions, include compounds of formula I or II, or pharmaceutically acceptable salts thereof, and pharmaceutically acceptable carriers that can effectively antagonize the action of cystoscin at their receptor sites 〇 The present invention also provides a method for treating or preventing conditions selected from mammals, including humans, pain, gastrointestinal disorders such as ulcers and colitis, and central nervous system diseases such as Jiaolian and fear, which include administration of Mammals are effective in antagonizing the amount of cystocystin at the receptor of the compound of formula I or I, or a pharmaceutically acceptable salt thereof. The compounds of formulae I and I have opposite palm centers and therefore have different enantiomeric and diastereoisomeric forms. The invention includes all optical isomers and all stereoisomers of compounds of formulae I and I, and mixtures thereof. The above formula I and formula I include the same compounds as described above, but in fact one or more hydrogen atoms or monatomic atoms are substituted by their isotopes. This compound is used as a research and diagnostic tool in metabolic pharmacy research and bond testing. DETAILED DESCRIPTION OF THE INVENTION The compounds of formulae I and I can be prepared as shown in the following reaction scheme and discussion. Unless otherwise stated, R7 and Z 2 in the following reaction scheme and discussion are as defined above. (Please read the notes on the f-face before writing this page) -Installation- Order_ -74. · This paper size is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -25-21B9Gi A6 B6 5 3 2 / IV clearly explain the schematic diagram 1

V Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs

N 丨 ci

X

(Please read the precautions on the back before filling out this page) _ _ order · · · 'spring · This paper standard applies to China National Standard (CNS) A 4 specifications (210 X 297 mm) 24) Schematic 2

A6 B6

(Please read the notes on the back before writing this page) (R1 = C02R2, R2 = Η)

—Installation. Ordering- (R1-CO, H) V4- Printed by the Ministry of Economic Affairs Central Bureau of Standards of Staff and Consumer Cooperation

t A CONR -27-This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) A6 B6 V. Description of invention (25) Schematic 3

(Please read the notes on the back before writing this page)

Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs

(R * = CO, R2, C6H5, CON R4R5 or S〇2N R3R6) The paper size is applicable to the Chinese standard (CNS) A 4 specifications (210 X 297 mm) -28-(i) Oi A6 B6 Central Ministry of Economic Affairs Printed by the Standard Consumer Engineering Cooperative V. Description of the invention (26) The preparation of the compound of formula I (hereinafter referred to as the compound of formula 1) of R1 SC〇2R2, C6H5, C0NR4R5 or S〇2NR3Re is shown in schematic diagram 1. Referring to schematic diagram 1, a compound of formula K reacts with hydroxylamine hydrochloride in methanol in the presence of 5K sodium bicarbonate or triethylamine to form a compound of formula IV. This reaction is usually carried out at a temperature from about room temperature to about the reflux temperature of the reaction mixture. The formed compound of formula IV is then reacted with tosylate helium in about 〇Ί〇 pyridine for about 24 hours to be converted into the compound of formula V. Alternatively, the compound of formula m can be directly converted into the compound of formula V according to the single-step method. According to this method, the compound of formula Π [NH2〇S〇3H (hydroxylamine-0-sulfonic acid) in formic acid reaction mixture at reflux temperature. This single-order method is superior to the second-order method for all compounds of formula IV except that γ / is phenyl and is adjacent to the gas group. Bromination of the compound of formula V produces the corresponding compound of formula VI. This bromination is generally carried out by adding a compound of formula V to a mixture of phosphorus pentachloride and pyridine in methylene chloride at about 01C. Alternatively, the second step, which includes adding a brominating agent, can be replaced by adding bromine at about ου and reacting it for about 0.5 hours to about 5 hours, preferably about 2 hours, to make a seven-membered ring containing saturated nitrogen Dibromide. It is then treated with hydrogen in the presence of a rake poisoned with quinoline to selectively remove one bromine atom. The brominated compound of formula VI is then present in tetrahydrofuran (THF) with sodium hydride. The formula XCHsR, where R1 is the base group, X is bromine and the other R2 are all bromine, react to alkylate the ring nitrogen. This reaction produces the corresponding compound of formula W, usually at a temperature of about room temperature to about 15 0 " 0. The paper size is applicable to the Chinese National Standard (CNS) A 4 specification (210 X 297 common potion) ~ 29 ~ (please first Read the precautions on the back and then this page) Installation _ Order--74. Printed A6 by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy ^-V. Description of invention (27). It is preferably carried out at the reflux temperature of the reaction mixture. The compound of formula VI formed in the above steps is then reacted with an alkali gold hydride compound to produce a compound of formula Vi. The preferred reactant is sodium nitride. Generally, this reaction is carried out in a reaction inert solvent such as dimethylformamide (DMF) or dimethylsulfoxide (DMSo), preferably DMF, at a temperature of about 60¾ to about 100t :, preferably about 80t: get on. Reduction of the azide of formula VI produces the corresponding amine of formula IX. This field is usually completed in the presence of Pd / C using a calendar of about 1 to about 3 atmospheres. Suitable reaction inert solvents include halogenated hydrocarbons and (C'_C6) alkanols. Ethanol is the preferred solvent. The reaction temperature is about 15 t: to about 70 t: preferably about room temperature. Alternatively, the reduction is carried out using trialkyl or triarylcarbohydrates. Examples of suitable reactants are triphenyl sulfonate and tributyl sulfonate. This reaction is usually carried out in a reaction inert solvent such as THF or another ether water-miscible solvent in the presence of water at a temperature of about room temperature to about 001C. Preferably, it is carried out in THF at about room temperature. The formed compound of formula IX is then converted to the corresponding compound of formula IA by reaction with an isogas ester of formula C ^ HeZiZ ^ NC 0. Suitable reaction inert solvents for this reaction include hydrocarbons such as hexane, benzene, and toluene, halogenated hydrocarbons such as digas methane and 1,2-digas ethane, ether solvents such as diethyl ether, THF and el y me, and pyridine. The preferred solvent is 1,2-difluoroethane or dichloromethane. Organic tertiary amines can be used as catalysts. The reaction temperature is about 0Ό to about 150 t :. The reflux temperature is better. The formula used in the above reaction C eH4Z2Z2NC 0 isocyanate is available (please read the precautions on the f side before writing this page) 丨 installed. Order_ 'Line · This paper standard is applicable to China National Standard (CNS > A4 ί 见 格(210 X 297 mm> -30-A6 B6 Printed by the Central Bureau of Economic Affairs of the Ministry of Economic Affairs, Shellfish Consumer Cooperation-V. Description of the invention (28) Formed by methods known to those skilled in the art. One method is included in organic bases Such as trialkylamine, preferably triethylamine or diisopropylethylamine in the presence of mixed benzoic acid derivatives and diphenylphosphoryl azide, or similar reagents. This reaction is usually in brewing, hydrocarbon or gasified hydrocarbon solvents , Preferably tetrahydrofuran or benzene, from about room temperature to about 1001C, preferably at the reflux temperature of the solvent, for about 20 minutes to about 24 hours, preferably about 1 hour. Scheme 2 illustrates that R1 in the formula is C. The compound of formula IA of 2R2 synthesizes the compound of formula I of Ri SC〇2H (hereinafter referred to as the compound of formula IB). Method. With reference to Scheme 2, the compound of formula IA in which R2 is C〇2R2 is hydrolyzed to produce the corresponding Acid of formula IB. Hydrolysis generally uses trifluoroacetic acid, in reaction inert solvents such as hexane, ether solvents (such as diethyl ether or THF) or halogenated hydrocarbons (such as methane or 1,2-dioxane), about one It is carried out at a temperature of 781C to about 501C. It is preferred to use trifluoroacetic acid in a halogenated hydrocarbon co-solvent at about OC. The acid of formula IB can be converted into the corresponding compound of formula IA by reaction with an amine of formula NHR4R5 in the presence of a dehydrating agent In the formula, it is C0NR4R5. The dehydrating agent is preferably a master diimine. Other dehydrating agents that can be used are 1,1 · monocarbonyl dimazole and isobutyl formate / N-methylmorpholine. This reaction is usually In the reaction inert solvent selected from hydrocarbons such as benzene, toluene and hexane, halogenated hydrocarbons such as methane and 1,2-dioxane, ether solvents such as diethyl ether, THF and glyme, and pyridine, preferably THF , About 0¾ to about 1201C, preferably about room temperature. (Please read the notes before filling out this page)-Binding · Order ·: 4. This paper size is applicable to China National Standard (CNS) A 4 Specifications (210 X 297 mm) -31-Printed by the Ministry of Economic Affairs, Central Standard Resident Employee Consumer Cooperative A6 B6 V. Description of the invention (29) Schematic diagram 3 illustrates the compound of formula I, where C〇2R2, C «Η C Ο NR 4R 5 or SO 2N R 3R β, (hereinafter referred to as the compound of formula IA). Reference diagram 3. The compound of formula X is converted into the corresponding compound of formula XI by the following two steps. First, the compound of formula X is converted into an oxime by the method of forming the compound of formula IV from the compound of formula Π as illustrated in schematic circle 1. Then the oxime is reacted with polyphosphoric acid The oxime is rearranged to form lactam of formula XI. The reaction is carried out at a temperature of about room temperature to about 20 Ot :. The reaction mixture is preferably heated to about 160 ° C. The formed compound of formula XI is then reacted with phosphorus pentachloride and pyridine, and then bromine is added to the bromide to form the compound of formula XI. The reaction with phosphorus pentachloride and pyridine is carried out as in the first step of bromination of the compound of formula V. The reaction with bromine, which forms monobromide, is carried out at about 781C to about 01C, preferably about -40C. Formula XI [The alkylation of the compound produces the corresponding compound of formula XI. Hospitalization is to make the compound of formula XI and formula XCH2R2, when Ri is phenyl, X is bromine and when only 1 is other group, X is iodine, react in the presence of lithium dialkylase in THF / DMSO . It is preferable to add DMS0 co-solvent after the addition of lithium dialkylzymidine. When the base is added, the reaction temperature is about −78 to about 0 °, preferably about −781C. When DMS0 is added, the reaction slowly returns to about _20t! To 50%. Preferably, when DMS0 is added, the reaction is warmed to about room temperature.

Use the above method to convert the formed compound of formula XI to the corresponding formula IA by the reaction sequence XV-IA shown in the schematic diagram 3. This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -32 ~ ---------------- 『-------- installed -------- order ----- ~ 4 (Please read the notes on the back before filling in (Clothing page) A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of the invention (3 °) The progress of the compound is similar to the reaction step shown in the schematic diagram VI-V dish · »I X- > IA The method is the same. The compound of formula I can be prepared by a method similar to the compound of formula I shown in schematic diagram 2, wherein, and the compound of formula I, where R 2 is C Ο NR 4 R 5〇 The raw materials used in the methods of schematic diagrams 1 and 3 or It is commercially available, or is known in the art or can be obtained from known compounds by methods known to those skilled in the art. The preparation of other compounds of formulae I and I that do not detail the above experimental part can be made using a combination of the above reactions as known to those skilled in the art. The pressures of the reactions described in the above schematic diagrams 1 to 3 are non-standard, unless otherwise stated. Generally, a pressure of about 0.5 atm to about 5 atm is acceptable, but the ambient pressure, ie about 1 atm, is easy to operate. The basic compounds of formulae I and I (active compounds of the invention) can form many different salts with various inorganic and organic acids. Although such salts must be pharmaceutically suitable for administration to animals, it is generally desirable to isolate the compound of Formula I or I from the reaction mixture with a pharmaceutically unacceptable salt, and then simply convert it to a free base compound by treatment with an alkaline agent, The free base is then converted into a pharmaceutically acceptable acid addition salt. The acid addition salt of the active base compound of the present invention can be easily prepared by treating the base compound with an inorganic or organic acid to be determined substantially in an aqueous solvent medium or an appropriate organic solvent such as methanol or ethanol. The solvent was carefully evaporated to obtain the desired solid salt. The active compound of the present invention and its pharmaceutically acceptable salts can be used as selective CCK-B receptor antagonists, that is, in mammals, the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) _ 33 — ---------------- ^ ------- installed ------, 玎 ----- (please read f first (Notes to be filled out again on this page) 21 V · 2 A6 B6 Printed by the Central Bureau of Standards of the Ministry of Economic Affairs, Labor and Consumer Cooperatives 5. V. Description of invention (31) The ability of the B-site of CCK to antagonize the effect of CCK, so it can be used as a treatment Therapeutic agent for sick mammals. The active compound of the present invention and its pharmaceutically acceptable salts can be administered orally, parenterally or topically. Generally, the most desirable dose of this compound is from about 5.0 mg to about 150 〇Bg daily, although the weight and condition of the snakehead to be treated depends on the route of administration chosen. However, it is best to use about 0.07 to about 2 1ag per kg of body weight per day. Of course, it may vary depending on the type of animal to be treated and its response to the drug, as well as the selected drug formulation and the time and interval of administration. In some cases, the dosage lower than the lower limit of the above range is more suitable, while in other cases, the use of larger doses still has no harmful side effects, as long as the larger dose is divided into several small doses in 1 day medicine. The active compound of the present invention can be administered alone or in combination with a scientifically acceptable carrier or diluent in any of the three routes mentioned above, and this single administration can be performed in a single dose or multiple doses. In particular, the therapeutic agent of the present invention can be administered in many different types, that is, it can be combined with various pharmaceutically acceptable inert carriers to form tablets, capsules, lozenges, tablets, hard candy, powders, sprays, creams, Ointment, column, jelly, gel, paste, lotion, ointment, aqueous suspension, injection, tincture, syrup, etc. Carriers include solid diluents or materials, sterile aqueous media, and non-toxic organic solvents. In addition, the oral hygienic composition can be appropriately sweetened and / or scented. Generally, the concentration of the therapeutically effective compound of the present invention in such a dosage form is from about 5.0% to about 70% by weight. For oral administration, lozenges containing various adjuvants such as microcrystalline cellulose, sodium citrate, calcium nitrate, dicalcium phosphate, and glycine can be used at the same time. ----------- installed ------ order ----- 14 (please read the precautions on the back before filling in this page) This paper size is applicable to China National Standard (CNS) A 4 Specifications (210 X 297 common patchouli) -34-A6 B6 Printed by the Employees ’Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs« V. Description of Invention (32) Disintegrating tablets such as starch (preferably corn, potato or cassava flour) And pending compound silicate, and granulation binders such as polyvinylpyrrolidone, sucrose, gelatin and gum arabic. In addition, lubricants such as magnesium stearate, sodium lauryl sulfate and talc are also extremely useful for granulation. A similar solid tar composition can also be used as a filler in gelatin capsules; preferred materials in this case also include lactose and macromolecular polyethylene glycol. When a suspension aqueous solution and / or elixirs are to be used as oral drugs, the active ingredient may be combined with various sweeteners or flavoring agents, colorants or dyes, and, if necessary, emulsifying and / or suspending agents and diluents such as water Combination of ethanol, propylene glycol, glycerin and various similar compositions. For non-gum administration, solutions of the active compound of the present invention in sesame or peanut oil or propylene glycol aqueous solution can be used. If necessary, the aqueous solution should be properly buffered (pH is preferably greater than 8) and first made into isotonic. Such an aqueous solution is suitable for intravenous injection. The oil solution is suitable for intramuscular, intramuscular and subcutaneous injection. Such a sterile solution can be easily prepared by methods known to those skilled in the art. In addition, the active compound of the present invention can also be administered locally when treating skin inflammatory conditions, and this can be accomplished with kits, jellies, gels, sorrels, oil threats, etc., according to Sassafras pharmacological experiments. The activity of the compounds of the present invention as C C K_B antagonists can be obtained by measuring the inhibitory ability of 125-I-BH-CCK-8 and CCK-B receptor binding in guinea pig skin formulations. This method proceeds as follows. A male Hartley guinea pig had its cortex excised and was tested in a 20-fold volume (w / V) test buffer, which included 50mH Τ Γ is (卽) trimethamine, 2 — amine group 2 — Xiangjia Base one (please read the note $ item on the back and then write this page) This paper A degree is suitable for China Sleepless Family Standard (CNS) A 4 specifications (210 X 297 mm) 1 35 _ .i A6 \ 韵 、. 二_B6_ Fifth, the description of the invention (33) 1, 3-malonyl fermentation) hydrochloric acid and 5mM chloride shovel, 4 homogenize with Teflon homogenizer under it (15 times). The homogenate was centrifuged at 41 and 100,000XG for 30 minutes. The pellets were resuspended in the same buffer and rotated as above. The final pellet is diluted with verification grade granules to a concentration of 20 ing / m ί for bonding test. The organization is kept on ice at all times. Prepare the incubation mixture, which includes the 50 w tissue formula prepared above, 100 0 u and 125-I-BH-CCK-8 (to produce a concentration of 50PM in the final test), 20wi blank or to be tested Compound, and Tr is 30 / ii with 4% DMS0. All drugs and dilutions were prepared using 4% DMS0 in assay buffer, resulting in a final assay DMS0 concentration of 196. Add the tissue to the 9 6-parallel plate containing 125-I-BH-CCK-8 and appropriate blanks and the compound to be tested to initiate the reaction. Use 1 WM sulfated CCK-8 to evaluate non-specific bonding. The reaction was terminated by rotating the plate in H 1 000B placed on a Sorvall RT 6000 refrigerated centrifuge 4 1C. Discard the supernatant, and the pellets are printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the "Notes on the back side and then * ^ page") • Ihua. 2 0 0 / ζί test buffer washing, The board rotates as above. Discard the supernatant again, use a Statron cell collector set at 2 2 2 on a Betapl-ate filter (which has been soaked in 0.2% polyethyleneimine for at least 2 hours), and use Tris PH7.4 HCP collects pellets for the wash buffer. The filtrate of each sample was counted on a Betaplate counter for 45 seconds. Data to I C 5. Value representation (inhibition of 50% of the original paper scale applies to China National Standards (CNS) A4 specifications (210 X 297 mm) -36-A6 printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs · B618U ^ r-- -5. Description of the invention (34) 125-1-BH — CCK — 8 specific bonding concentration). Use nonlinear regression analysis to analyze the data. The following examples illustrate the invention. However, it is known that the invention is not limited to the details of such examples. Example 1 N — Third Ding 2 — Γ3- (3 — (3 — Jiaben) Urea) 1 — 2 — M — 5 — Rong 2 2. 3. 4. 5 — Tetraargon-1H 1 (1) Fuyou argonine-1 1] Acetamide A. 3 —Bromo-5_ Rongmou—2. 3. 4. 5 — Siqiyi 1 Η — (1) Fen and gas mixed leather-2 -The ketone contains PC ί 5 (1.041g, 5mm〇l) dissolved in 5 Om ί dichloromethane in a 125m round bottom flask and add 5-phenyl-2, 3, 4, 5 in an ice bath under nitrogen , —Tetrahydro-1H (1) benzodiazepine-2-one (1.187g, 5 »m〇l). It was observed that the temperature increased slightly, and pyridine (〇 · 42mi ?, 5.25mB〇l) in 5mj? Dihelium was added dropwise quickly. The mixture was stirred for 15 minutes and then cooled to 45¾. Then, bromine (0.258mi, 5 mmol) in 7mi2 dichloromethane was added dropwise with rapid stirring for 30 minutes. After 15 minutes the bath was removed and the mixture was warmed to room temperature. Thin layer chromatography (TLC) (silica gel, 33: 2 dichloromethane: ethyl acetate) showed no raw materials, only non-polar intermediates (kimo-imino). The residual reaction was diluted with an equal volume of tetrahydrofuran and 200 rn? Water was added. The size of this mixture is not based on the Chinese National Standard (CNS) Grade 4 (210 X 297 mm) ~ 37 ~ (please read the note before filling in this page). Order-iline · Central Standard of the Ministry of Economic Affairs Printed by the Bureau and the Industry and Consumer Cooperative Society A6 ^ 13901 _ ^ _ V. Description of the invention (35) Stir for 40 minutes and then separate. The aqueous layer was re-extracted with dichloromethane and the combined organic fractions were washed with water, dried with brine and sodium sulfate, filtered and evaporated to produce 1.56g (98.7%) of unprocessed product. The diastereoisomeric bromide (R / = 0.57 and 0.48) can be separated by chromatography or crystallization from ether and hexane; however, the mixture is directly used in the next step (B). The solids obtained by crystallization are mostly more polar isomers, and the mother liquor contains less polar isomers and trace amounts of gaseous imines and raw materials. The more polar diastereomers recrystallized from chloroform to produce large crystals, mp 191-1921C: 2H-NMR (δ, CDCla): 2.92 (m, 1H), 3. 1 4 (m, 1 H) , 4. 4 9 (m, 1 H), 4.63 (m, lH), 6.77 (d, lH), 7. 09 (m, 3H), 7. 32 (m, 6H), 7.85 (bs, lH) 〇MS (%): 315/317 (parental Br79 / Brei, 20/18), 236 (78), 208 (100), 194 (3 6), 1 8 0 (7 3), 1 3 0 (4 7), 1 1 5 (3 9), 91 (7 9) 〇B. 2-[3-bromine-2-argon-fS-Zhu a certain 2. 3. 4, 5-tetrahydro-1H-(1 ) Rong # Xenon miscellaneous cocoon 1—some 1 ?! Three third butyl ester in a flask with a partition and N2 inlet 1 25111) 2 three-necked round bottom flask (please read the notes on the back and fill in this page)丨 Installation · Ordering--4 · The standard of clothing paper is in accordance with the Chinese Standard B (CNS) Grade 4 (210 X 297 public) -38-

6 B Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of invention (36) Add 3-bromo-5-phenyl-2, 3, 4, 5, 1, tetrahydro-1H (1) benzo under nitrogen Krypton mixed leather 2-one (3.216g, 10.17m «ol) and 50mi? Anhydrous tetrahydrofuran (THF). The reaction was cooled in a dry ice bath, and lithium bis-trimethylsilylamide (11.2 ml of 1MJ in THF) was slowly added. The mixture was stirred for 5 minutes. Then add the third butyl iodoacetate (2.708g, 11.19miB〇l) 0 remove the bath and add 25mi dimethyl sulfoxide (DMSO) at 20 * C. After 1 hour at room temperature, TLC (24: 1, CH2Cl2: EtOAc) showed only a slight amount of starting material in the acidified portion. The reaction mixture was poured into ice water and ethyl acetate containing 25 mi? N. H C i ?, stirred for 5 minutes and separated. Repeated ethyl acetate extraction and the combined extracts were washed several times with water, dried with brine and sodium sulfate, filtered and evaporated to produce 4.9 g (> 100%, still containing traces of solvent) unprocessed product. Similarly, the internal aldol is alkylated with N-third butyl iodoacetaldehyde amine to produce N-third butyl 2- [3-bromo-2-gas-1 5-phenyl-2, 3, 4, 5, —tetrahydro-1H (1) benzodiazepine-1-yl] acetamide. C. N — third butyl “3 — azide — 2 — argon — Rong certain 2. 3. 4 ·. 5 — four gas one 1H — (1) Rong and 氤 hetero group — 1 mono] Acetyl acetate In a 25OmJ? Round bottom flask equipped with an N2 inlet of an amine, add N —third butyl 2_ [3 —bromo-2_oxo 5 —phenyl-2, 3, 4, (please read the precautions on the back (Fill in this page again) i Pack · Order.: 4- This paper scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 2 mm) -39-Ministry of Economic Affairs Central Oak Quasi I® Industrial and Consumer Cooperation Duin System A6 21 ^^ 01 _ ^ _ 一 五. Description of the invention (37) 5, -tetrahydro-1H (1) benzoazepine leather; ι monoyl] acetamide acetate (8.317g, 19.37 〇1 ), 90mJ? Dimethyl formaldehyde amine (DMF), and * sodium nitrate (5.25g, 80 Zu Diao 〇1), under cyanide), the mixture was heated at 751C »20 hours. Then the reaction mixture was cooled Disperse between water and ethyl acetate, separate, and then extract the aqueous phase. The combined extracts are washed three times with water, hydrogen peroxide solution once, then dried with brine and sodium sulfate, filtered and evaporated, leaving a gummy residue, 8. 58g (100%), with a little solvent .; H-NMR (δ, C DC13): 1.48 (s, 9H), 2. 88 (m, 2H), 4. 52 (AB quadruple, J / ie = 17, = 138, 2H), 4. 57 (m .1 H), 5. 06 (m, 1 H), 6. 73 (d, 1 H), 7.26 (m, 8H) 0 D · N-the second Dingmou 2 ~~ [3 monoamine even — 2 — gas one 5 one Benji-1 2. 3. 4, 5 — Tetsushin-1H — (1) Rong # Xenanza-1—1 xyloamine 1 Unprocessed product from the above substitution reaction, N—third butyl 2 A [3-azido-2-gas-5-phenyl-2,3,4,5, -tetrahydro-1H (1) benzodiazepine-1 1-yl] acetamide, (8 · 58g , 19. 37 ^ 0 1), dissolved in 75m) 2 methanol under nitrogen. Added catalyst, 6g 5% Pd / C, 50% w / w, the mixture was hydrogenated at 55p si H2 for 5 hours. The mixture was filtered through Celite®, the catalyst is washed three times with formazan and the filtrate is evaporated. TLC (This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 public goods)) 40 — ---------- ------ ^ ------- installed ------ order ----- 14 (please pay attention to the Mf surface first and then buy it in Evo). Printed by the industrial and consumer cooperative ^-V. Description of the invention (38) 24: 1, dichloromethane: methanol, silica gel) display The low-polarity material and product R / = 0. 25. The raw product was tweezed into ethyl acetate and extracted with acid. The acidic extract was refluxed with ethyl acetate, and the aqueous phase was taken in new ethyl acetate and the pH was adjusted to 10.0. The organic fraction was dried with brine and sulfuric acid, filtered and concentrated to produce 1.832g (25.8%) of crystalline amine (mp 189-192TC, diastereoisomer). The mother liquor produced 1.545g (21.8%) of foam after stripping the solvent, which contained a nearly 1: 1 mixture of diastereomers. 2H-NMR (δ, CDCh): 1.30 (s, 9H), 2.2 (bs, 2H), 3.06 (AB quadruple, Jas = 15, = 276, 2H), 2.67 (m, 1 Η), 2. 84 (m, 1 Η), 3.57 (m, 1 Η), 4.18 (m, 1H), 6.01 (bs, 1H), 7.2 (m, 9 Η) 〇E. N-玮 三Butyl 2_ "3 — (3-(3_ 申 荣 某) urea) -2 —hydrogen 5 —benzene 2 2. 3. 4. R —tetrahydrogen 1H_ (1) juxenoxan (1 一 某) Ethylenediamine A 251115 round bottom flask equipped with an Ns inlet was charged with N-third butyl 2- [3-amino-2-pyridine-5-phenyl-2,3,4 under nitrogen , 5, —tetrahydro-1H (1) benzodiazepine-1-yl] acetamide (0. 50g, 1. 368mm〇l) and i〇mi? Two gas methane, the reaction was cooled in an ice bath . Then add m-toluene isopentanoate (◦. 194mi ?, 1. 5 «a〇l) in 5m5 dichloromethane drop by drop China National Standards (CNS) A4 specifications (210 X 297 common patchouli) 41 A6 __ ^ V. Description of the invention (39). A solid is formed immediately. Continue stirring for 15 minutes, then remove the ice bath and return the reaction to room temperature Hours. Filter out solid "And washed with dicyanomethane / hexane (1: 1) to produce 600« g (87.9%) product, mp 263-266 * 0. 2H-NMR (δ, DMSO-de): 1. 2 3 (s, 9 Η), 2. 21 (s, 3 Η), 2. 54 (m, 1 Η), 2.9 (m, 1H), 3.34 (AB quadruple line, J λ 1 6, Δ, = 255 , 2Η), 3. 4 (HOD spike), 4. 34 (m, 2Η), 6.8 (m, 2Η), 7.3 (m, 11H), 8.78 (s, lH). Use the same as in Example 1 Method to prepare the target compounds of Examples 2 to 10. Fen Yuan Example 2 2-[3-(3_ (4-gas phenyl) adenyl)-2-gas-5- cyperyl-2. 3.4. 5-four 氤1 1H— (1) Rong Fan Tan j Zashen-1 1 Yimou 1 ethyl ash tributyl _ chromatographic and crystallization yield 30%, M.P. 148 — (please read the precautions on the back side first (Write this page) • Installed • Printed by the Ministry of Economic Affairs, Central Standards Bureau, 8 Industrial and Consumer Cooperatives 1 5 0 1C 〇7 Η--Ν Μ 1 R (δ, CDC 1 3) • 1 • 3 7 (S t 9 Η ), 2. 8 — 3. 1 (m, 2 Η) 9 3 • 3 0 (A Β quadruple, ϋ Λ Β = 1 7, Δ ν = 1 8 8, 2 Η) 9 4 • 2 7 ( m, 1 Η), 4 .7 6 (m, 1 Η) »6 • 8 (width s 9 1 Η), 7 .0 a 7 • 5 (m > 1 4 Η) ο MS (96): 520 (18, parent), 366 (35 -42-This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) Employee consumption of Central Bureau of Standards, Ministry of Economic Affairs A6-1 Β6 printed by the cooperative ---- V. Description of the invention (40)), 3 3 7 (4 3), 2 6 7 (7 0), 2 0 6 (8 5), 1 5 3 (7 6 ), 1 2 7 (1 0 0), 91 (53). HRMS calculation C mH hN 301: 520. 2003. Experiment: 520. 1983. Example of Fen Lu 3 N — the third Ding 2 — “3 — (3 — (3 —Xing Rong) ureido) one 2 —argon one 5 — stupid one 2. 3. 4. 5 — four gas—1H One (1) —Rongyou Zhazai-1—A certain 1 ethyl acetamide produced 90% yield, mp 264-266t: ^ -NMR (δ, DMSO-di): 1.21 (s, 9 Η) , 2. 56 (m, 1 Η), 2. 9 (m, 1 Η), 3. 3 5 (AB quadruple, JxS = 17, Av = 255, 2 H), 4. 37 (m, 2 H), 6.7-7. 6 (m, 14H), 9.08 (s, lH) MS (%): 518 (1, parent), 322 (40), 194 (60), 91 (70) , 58 (l〇0) o HRMS calculation C 3iN 4〇1: 518. 2097. Experience: 518, 210 0. Fen Shi Example 4 N — third butyl 2 — “3- (3- (3--A Rongmou) urea group) — 2 — Atmosphere 5 — Juki — 2. 3. 4. 5 — Tetraargon — 1H — (1) Ju and 氤 杂 箪 _1 一 某] acetoxamide—— ------------ (------- installed ------. 玎 ----- ^ 4 (Please read the notes on the back before writing this page) This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -43-Printed by the Employees ’Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 2Χ39〇 ^ B6 V. Invention Description (41) 85% yield, mp 2 3 1-2 3 3 t: 〇 ^ -NMR (δ, CDCla): 1.28 (s, 9 Η), 2. 2 4 (s, 3 Η), 2. 65 (m, 1 Η), 3.09 (AB quadruple line, JAB = 17, / iw = 291, 2 Η), 3.11 (m, 1 Η), 4.22 (m, 1 Η), 4.62 (m , LH), 6.011 s, lH), 6.41 (width s, lH), 6.9-7.5 (m, 1 3 H) MS (96): 498 (0.5, parent), 322 (5) , 2 9 4 (8), 133 (8 0), 105 (1 0 0), 7 8 (8 0) 〇HRMS calculation C 3〇H hN 4〇3: 4 9 8. 2 6 3 0. Experiment: 498. 25475. Example 5 N—Third Butyl 2— “3— (3- (3- (3- (Shenyi-Phenylphenyl) ureido) -2—Argon 5—Rong 2.2.3 4. 5-Tetral_1H- (1) Benzene Gas Leather 1-1] Yieldamine Acetate 81% yield, mp 254-25710. 1 Η-NMR (δ, DMS0-d «): 1. 21 (s, 9H), 2.56 (m, lH), 2.9 (m, lH), 3.3 3 (AB quadruple, Ju = 16, = 259 .2 Η), 4.35 (m, 2 Η), 6.4-7.6 (m, 14H), 8.865 (width s, lH) 0 ---------------- ^- ------ Install ------ Order ----- (Please read the precautions on the back before writing this page) This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 Mm) -44-A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs

5. Description of the invention (42) MS (96): 514 (0.1, parent), 322 (6), 149 (100), 106 (40). HRMS calculation CaoHHNiOi: 5 14. 2553. Experiment: 514.26134. Example 6 N—Third Dingmou 2— “3-(3-(4-Ningrong) urea) —2 —Gas—5 —Benji-1 2. 3. 4. 5 — Tetraargon-1H-1 (1) Juxenon xenon cocoon-1 1 Ί Z Zyzolamine 88% yield, mp 247-2491C. ^ -NMR (δ, CDCl ^): 1.31 (s, 9 H), 2. 92 (m , 1 H), 3. 10 (m, 1 H), 3. 2 2 (AB quadruple line, JxS = 16, Z \ p = 260, 2 H), 4. 29 (m, 1 H), 4 . 60 (m, 1 H), 5.74 (width s, 1H), 6.43 (width s, 1H), 7.0-7.5 (m, 13H) MS (96): 518 (1, parent), 322 (40), 261 (7〇), 153 (100) o HRMS calculation C29H3iN4〇3Cl: 518.2070. Experiment: 518.21007. Fen Shi Example 7 N — Qiu Sanding 2 — Γ3 — (3 — (4 — Jia Rongmou) urea) one 2 — gas one 5 — stupid one 2. 3. 4. 5 — four gas one 1H (please read the note on the back first and then write this page) 丨 Install · Order- ▲ This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -45-213901 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (43) One (1) Xenon-hybrid-1—a certain] acetamide acetate 95% yield, mp 235-2381C. ^ -NMR (δ, CDCla): 1.29 (s, 9H), 2.27 (s, 3H), 2.72 (m, 1H), 3.12 (m, lH), 3.25 ( AB quadruple line, Jjis — 16 »Δι / = 283, 2Η), 4. 24 (m, lH), 4.6〇 (m, lH), 5.88 (width s, lH), 6.8-7.4 (m, 14H) 〇MS (96): 498 (1, parent), 322 (30), 2 4 9 (1 5), 221 (2 0), 194 (2 0), 1 3 3 (1 0 0) 〇HRMS calculation C3〇H34N4〇3: 498. 2646. Experiment: 498. 26153. Fen Shi Example 8 N — the third Dingmou 2 — Γ 3 — (3-trifluoromethanone Rongmou) urea) one 2-gas-5 -Benyl-2, 3. 4. 5-Siqi-1H- (1) Mo-tritium heterodione-1-yl-1 acetamide yield 67%, mp 135-1391C. 2H-NMR (δ, CDCla): 1. 3 0 (s, 9H), 3.1 (m, 2H), 3.31 (AB quadruple, = 16, Δ, = 270, 2H), 4-32 (m, 1 H), 4.62 5.77 (width s, lH), 6.6 (width s, lH), 7.0-7.9 (m, 13H) o This paper scale is applicable to the Chinese National Standards (CNS) A 4 specifications (210 X 297 mm ) —46 — (Please read the precautions on the back before writing this page) 〇1E9〇1 A6 B6 Printed by the Ministry of Economic Affairs Central Standard Resident Consumer Cooperative Co., Ltd. V. Description of Invention (44) MS (96): 552 (0. 2, parent), 416 (1), 3 2 2 (5), 2 5 4 (2 0), 91 (1 0 0) 〇HRMS calculated C3cH3iN4〇3F3: 552.2341. Experiment: 552.2288. Fen Shi Example 9 N — the third Dingmou 2 — Γ3 — (3 — (3 —thiomethan urea) urea) a 2 -gas —5 —Stunyl —2.3 3. 4. 5 —four gas― 1H— (1) 笨 #Xenon hybrid leather—one-one 1 ethylacetamide 78% yield. 2H-NMR (δ, CDC13): 1.22 (s, 9H), 2.35 (s, 3H), 2.58 (m, 1H), 2.97 (m, 1H), 3.21 (AB quadruple , J "= 16, = 288, 2H), 4.18 (m, 1 Η), 4.40 (m, 1 Η), 6.6-7.4 (m, 13H), 7.75 (width s, lH), 8.67 (Wide s, 1 Η) 〇MS (96): 530 (0.7, parent), 322 (18), 261 (21), 165 (100), 132 (32) 〇HRMS calculation CwHwNiOaS: 530.2352 .Experiment: 530.2332. Fenshi Example 1 0 2 — [3 — (3 — (3-benben) urea group) —2—argon—a paper scale applies the Chinese National Standard (CNS) A4 specifications (210 X 297mm) One 47 (please read the precautions on the back before writing this page) 丨 Installation_ Order_ 『4- A6 B6-Fifth, the description of the invention (45) 5 Two ^ base one 2_ 丄 ^ 3 · 4 · 5 — Four values one 1H — (1) Rong # xenon leather .. a 1 _ one base Ί 7, acetic acid third Ding Ku 76% yield, mp 1951C. 2H-NMR (δ, CDC13): 1.4 (s, 9 Η), 2.29 (s, 3H), 2.72 (m, lH), 3.19 (m, lH), 3.28 (AB quadruple line, J "= 16, = 230, 2H), 4 . 22 (m, 1H), 4.7 (m, lH), 6.37 (width s, lH), 6.78-7.5 (m, 14H) 〇MS (96): 500 (18, parent +1) , 484 (4) .444 (20), 426 (4), 337 (42), 311 (1 0 0), 2 6 6 (2 0), 2 4 0 (3 0), 194 (34). Example 1 1 3 ~~ (3 —Methylbenzyl gland) * 7— ~ Some one (N ~~ (N —2-Adamantyl) carboxylamine amine Shenshi) Six-value gas mixed leather-1 2 — Ketone A. 7—Phenylhexahydrogen mixed M—2—ketone equipped with 2 inlets of Ν2 2 5 0 mi? Figure bottom flask was added 7. 33 g (38. 8n »aol) 2 — phenylcyclohexime (Che .. Ber .. 55, 3664 (1922)) and 25mi? Pyridine. The solution was cooled to zero, and 9.61 g (50.4 mmol) of p-toluenesulfonaldehyde atmosphere was added. The reaction was stirred overnight under ice melting and then poured into water. Excess nitrogen was removed from the surface, and the reaction mixture was stirred at pH 4 for 3 hours. Filter out the precipitate (please read the precautions on the back before writing this page) 丨 installed. Ordered Γ4 The paper printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs is again applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) 1. 48 A6 B6 5. Description of the invention (46), washed with water, dried to a solid, 4.65g (55%), mp 1 3 5 — 1 3 7¾ (J · Am · Che ·. Soc ·. 8 2 · 4 6 7 1 (1960) produces mp 1 3 9-1 4 1 1C) The Central Standards Bureau of the Ministry of Economic Affairs 8 Industrial and Consumer Cooperation Du Printed B. 3 — Gangyi 7 — Duanyi 16 Qi Qi Zhuan Yi 2-Que 250ml round bottom flask equipped with N2 inlet was added 5.12 g (24. 6 mmol) phosphorus pentachloride and 45mi? Dimethane. Cooled to Ot: The stirred mixture was added dropwise 4.65g (24.6m «〇l) 7-phenyl-hexahydroazazepine-2-one and 3.98ιηβ (49. 2» test. 1) A solution of pyridine in a 40-meter second-dimension nail salon. Ot: Next, 9.25 g (24.6 mm〇l) of phenyltrimethylammonium bromide was added to the stirred mixture. The reaction was then warmed to room temperature and stirred for 3 hours. It is then evaporated, taken in tetrahydrofuran, quenched with water, evaporated, and distributed between water and methane. The organic layer was washed with water and washed with saturated aqueous sodium bisulfite solution, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel using ethyl acetate / hexane as the eluent to produce an oily product, 4.0 g ( 6 1%) ^^ NMR (δ.CDCl ^): 1.8-2.4 (m, 6H), 4.35 and 4.63 (multiple lines, 1H), 4.7-4.9 (111, 11 ^, 5.73 and 5.81) (Wide single line, 1H, NEJ, 7.2-7.4 (m, 5H). IR (cm-2, CHCla): 1 6 7 0 (C = 0) MS (96): 267 (6, pro Generation), 188 (39), 160 (70), 106 (100), 91 (43), (please read the $ surface note $ item first and then this page) _Installed · Ordered-ϊ4_ This paper is also suitable for China The national quasi-quasi (CNS) A 4 specifications (210 X 297 public potion) -49 A6 printed by the employee consumer cooperative of the central standard of the Ministry of Economic Affairs --- V. Description of invention (47) 5 5 (5 9) 〇C. 3— Tongyi 7-Zhu Mou (N-Chong Sanding) and a six-gas gas mixed with a 2-ketone in the OOmi three-necked round-bottom flask equipped with Nz inlet was added 0. 30g (6. 07 mmol) hydrogenated sodium, which was washed with hexane and suspended in 3mi anhydrous tetrahydrofuran. The stirred mixture was added dropwise 1. 55g (5.78mm〇l) 3-Mo a 7 in 20 minutes -A solution of phenyl hexahydroazaza-2-ketone and 1.4 2 g (6.07 mmol) iodoacetic acid tert-butyl ester. The reaction was stirred at room temperature for 3 hours to saturate an aqueous solution of vaporized ammonium It was quenched and taken in ethyl acetate. The organic layer was washed with water and brine, dried with sodium sulfate, and evaporated. The residue was analyzed on the simulant using ethyl acetate / hexane as the eluent, resulting in oil. Product, 1.65g (75%) 〇 ^ -NMR (CDC13): 1. 40 and 1. 42 (single line, (H, two diastereomers), 1.8-2.4 (m, 6H) , 3. 6-3. 9 (m, 2H), 4. 56 and 4. 95 (multi-line, 1H), 4. 71 and 5. 16 (multi-line, lH), 7.2-7.4 (m, 5H) 0 D. 3-Musk Xenon 7-Zhu Mou (N-butane carbonylmethyl)-6 Μ 鰤 mixed leather-2-ketone equipped with Ν2 inlet l〇0mP squat flask was added 1. 65 g ( 4. 32mm〇l) 3 — Moyi 7 — Phenyl I (N — third butadiene gas This paper standard is applicable to China® Home Standard (CNS) A 4 specifications (210 X 297 mm) -50 (please read the back (Please fill out this page again) —Installation · Order · -74 · A6 B6 Printed by the Consumer Labor Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 3. Description of the invention (48) Carbonylmethyl) hexahydroazaza-2-one, 4mi dimethylformamide, ◦ · 3 4 g (5.18 mmo 1) sodium azide, and 1 drop of water . The mixture was heated at 80 ° C for 36 hours, poured into water and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulfate and evaporated. The residue was chromatographed on silica gel using ethyl acetate / hexane as the eluent to produce an oily product, 1.0 g (67%). 7H-NMR (δ, CDCla): 1. 3 4 (s, 9H), 1 · 7-2. 4 (m, 6H) (only one diastereomer can be accurately determined), 3.6 2 (AB quadruple, Jm = 17, Δ, = 193, 2H), 4. 38 (m, 1 Η), 4. 77 (m, 1 Η), 7. 2-7.4 (m, 5H) 〇 IR (cm-1, KBr): 2106 (1 ^) and 1739 and 1661 (C = 0) 0 E... S-amine xenon 7-Rongmou _ (N-羮 三 丁 argium americium a certain field) a Liuqiqizaixi 2-brewing the azide (6.10g, 2.19 mmol) from the above step D in the presence of 2 0 0 mg 10% sulfonate rake in 30 m ethanol at 45 ib / i η2 Hydrogen treatment for 4.6 hours. The reaction was filtered through Celite® and evaporated to leave oil, which was used directly in the next step. 2H-NMR (δ, CDCla): 1.6-2.4 (m, 6H), 3. 63 (only one diastereomer can be confirmed) (AB quadruple, Jw = 17, = 156, 2H), 4 . 0 2 (m, 1 Η), 4. 9 1 (m, 1 Η), (please first read the note $ item and then f this page) i pack. Order _ i line, the paper size is applicable to the country Standard (CNS) A 4 specifications (210 X 297 mm) -51 〇1 B6 V. Description of the invention (49) 7. 2 — 7. 4 (m, 5H) 〇

IlMcm-1, pure): 1741 and 1649 (C = 0). F. 3 — (3 — A stupid man sleeps very much 1 1 7 — Mo one (N — flute tributane gas methyl group) a six-value gas heterogeneity Μ 2 — Gu loaded into the 〇2 entrance of l〇〇mi 1.28 g (4.02 mm〇l) 3-amino-1, 7-phenyl- (N-third butoxycarbonylmethyl) -hexahydroaza- 2-ketone, 5mL was added to the round-bottom flask 1,2-dichloroethane and 0.5 7m ί (4.43 mmol) 3-tolyl isocyanate. The reaction was stirred at room temperature for 3 hours and chromatographed on silica, using ethyl (please read the back side first (Notes to fill out this page) The Ministry of Economic Affairs Central Standards Bureau employee consumer cooperatives printed ethyl acid / hexane as an eluent t produces an oily product 0 This oil is crystallized from isopropyl ether to produce a solid, m P 1 9 4 — 1 9 6 t: o 2H--NMR (δ, CDC 1 i 3); 1 • 2 5 (sf 9 Η) 9 1 .6-2 ♦ 3 (m > 6 H) »2» 1 7 and 2 « 2 0 (single peak t 3 H »(diastereomer) t 3« 5 6 (A Β quadruple, JAB = 1 7 »△ V = 2 3 6 t 2 Η) t 5» 0 1 ( d, J = 1 1 »1 H)» 5 • 0 8 (m 1 H) f 6 • 7 1 (d 9 J = 7 t 1 H) 6 • 8 —— 7 ♦ 3 (mf 9 H), 7 ♦ 8 7 (sf 1 H) IR (cm -2 f KB r) • 1 7 4 3 and 1 6 5 0 (C = 0) 〇M s (%) • 4 5 1 (1 4 f parent) t 1 5 9 (4 5) 9 1 1 7 (6 4) t 1 0 7 (1 0 0) t 9 1 (4 6), 57 ( 41), 56 (48). The paper size is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 g; *) -52 A6 A6 213Q01 B6_ V. Description of the invention (50)

Analysis and calculation of C 26H33N3O4: C, 69. 16; H, 7.57; N, 9.31. Experiments: C, 6 9. 1 Ο; Η, 7. 75; N, 9. 08〇G. 3-(3-tolyl ureido)-7-Tsu a certain (N-carboxymethyl) six gas Gas mixed leather 2-Que 100mL round bottom flask equipped with Ν2 inlet was added 1.5g (3.3 2 mmol) 3- (3-tolyladenyl)-7-phenyl one (N-third butyl Gas carbonylmethyl) hexahydro aza leather 2- ketone and 25 mi of two gas methane. The solution was cooled to 0t: and 5mi trifluoroacetic acid was added. The reaction was then stirred at ου for 1.2 hours. The reaction was poured into water, extracted into methane, the organic layer was washed with water and brine, dried over sodium sulfate, and evaporated. The residue crystallized from isopropyl ether to produce a solid. ^ H-NMR (δ, CDCla): 1.4-2.2 (m, 6H), 2.22 and 2.24 (single peak, 3H (one for each diastereomer)), 3.5 5 and 3 . 6 1 (AB quadruple line Jxs = 18i Δι. = 138 and AB quadruple line-2, J αβ = 18, △! / = 348, 2Η), 3.4-3.8 (m, lH) , 4.0-4.1 (m, lH), 6.6 and 6.78 (m, 2H), 7.07-7. 4 (m, 9H) 〇IR (cm-1, KBr): 1740 and 1640 (C = 0 ) 〇 MS (%): 395 (9, parent), 159 (63), 133 (100), 98 (78) 〇 (please read the remarks on the back before filling in this page) i install · order · economy The paper printed by the Ministry of Standards and Staff's Consumer Cooperative applies to the Chinese national standard (CNS> A4 specifications (210 X 297 publication)> -53 A6 B6 Printed by R Industrial and Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy-V. Description of invention ( 51) HRMS calculation C22H25N3〇4: 395.1 769. Experiment: 395.1853. Η. 3-(3-methacrylonitrile)-7-Zhu certain (N-f N-2-adamantyl) carboxyl sleep Amine Shenshi) Hexaargon xenon mixed leather 2 — aa Add 330 m (0.83 5 mi »〇l) in a 100m5 round bottom flask equipped with an N2 inlet 3 — (3-tolylurea) 7 —Phenyl— (N —carboxymethyl) hexahydro Krypton leather 2-ketone, 5 mj? 1, 2-difluoroethane, 0.25g (1.7. · 〇1) 2-amine fund Gangdamane, and 0.24 g (1.25 mmol) ethyl (dimethylaminopropyl) bis-imine. The reaction was stirred at room temperature for 3 days and chromatographed on silica gel using methanol / dichloromethane As an eluent, an oil is produced, which crystallizes from isopropyl ether to produce a solid, 20% (4.5%), mp 14 5-153, 0 2H-NMR (δ, CDC13): 1.4-2. 2 (m, 22Η), 2. 20 and 2. 23 (single peak, 3Η, one for each diastereomer), 3.6 (AB quadruple, JAe = 14, = 121 (only one group, other groups Fuzzy), 2H), 3. 9 (m, 1H), 4. 5-4. 8 (m, 1H), 5. 04 and 5. 12 (multiple lines, 1Η), 6. 08 and 6. 4 2 (d, J = 8, 1H), 6.7 and 7.0-7. 4 (m, 9H), 7. 65 and 7. 77 (m, 1 Η) IR (cm-1, KBr): 1650 ( C = 0). MS (96): 528 (6, parent), 193 (100 (please read the precautions on the back and then write this page) i Pack-Order · This paper size is applicable to the national standard (CNS> A4 specifications ( 210 X 297 mm> -54, heart A6 21 2 ΰ d___B6_ V. Description of the invention (52)), 1 7 1 (6 5) 〇HRMS calculation C32H4 <) N4〇3: 528. 3 1 00. Experiment: 528 3051. Analysis and calculation of C η Η 4. N 4 0 3 · 0.5 Η 0: C, 71. 48; H, 7. 69; Ν, 10. 42. Experiment: C, 71. 61; H, 7 34; N, 10. 2 7 〇 Example 1 2-2 1 The target compound was prepared using the same method as Example 1 1. Fen Shi Example 1 2 3-(3 a rongrong gland a) a 7-base One (N_Third Ding (please read the note on the back first and then write this page) 氤 carbonyl a certain Shen Shen) one six 氲 Xenon Heterophthalmide 2 _ 79% yield, Μ. P. 75-861 2H-NMR (δ, CDCla): 1.3-2. 1 (Multiple lines of continuous ore t 6 H printed by the R and Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs) * 1 • 4 4 (s reference 9 Η), 2 • 2 9 (S 9 3 Η) t 2 • 7 a 3 • 2 (m ref 2 Η) $ 4 • 0 5 (AB 9 JAB = 1 7 9 △ V = 6 6 »2 Η) > 4 * 2 — 4 3 (mt 1 H) f 5 • 0 5 (m > 1 Η) »6 • 8 — 7 • 5 (mt 1 1 H) 0 13 C-NMR (δ f CDC 1 3): 2: L · 5 , 2 8 • 0 f 3 2 • 2 t 3 9 • 7 f 4 5 • 2 9 5 2 «3» 5 8 • 4, 8 1 • 9, 1 1 7 • 1 2, 1 2 0 • 8 t 1 2 7 • 0 f 1 2 8 ♦ 8 t 1 2 8 9 9 f 1 3 7 • 1 t 155, 168. 7, 175, (Not all aromatic amines are included in this paper scale. China National Standards (CNS) A4 specifications (210 X 297 mm) -55 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy ... A6 0.130 ^ 1_Be_ V. Description of Invention (53) Scan). MS (96): 465 (9, parent), 374 (17), 185 (6 6), 170 (61), 107 (100), 91 (64), 83 (43), 57 (58 ) 〇HRMS calculated C26H〇N304: 465.25933. Experiment: 465.26576. Example 1 3 3— ((3-Aminophenyl) ureido) 7—ring B group 1 (1 1 (please read the note on the back first and then write this page) Didibutyrium Some) a six argon xenon mixed leather 2__ 87% yield, mp 7 5-8 4 t: 〇2H-NMR (δ, CDC13): 1.3-2. Continuous multiple lines, 6 Η), 44 (s, 9H ), 2.7- 3.2 (m, 2H), 4. 06 (AB, J λβ = 1 7, Δ „= 62, 2Η), 4. 2-4.3 (m, 1Η), 5. 0 5 (m, 1H), 6. 9-7. 6 (m, 1 1 Η) MS (96): 485 (1, parent), 394 (22), 3 3 8 (2 3), 3 0 3 ( 3 4), 185 (1 0 0), 170 (76), 127 (90), 91 (73), 57 (74), 56 (80). HRMS calculation C26H37N3〇4F3: 485. 20929. Experiment: 485. 20705. The size of the bound spring paper is applicable to the National Standard (CNS> A4 specifications (210 X 297 mm) -56 V. Description of the invention (54) g Example 1 4 Α6 Β6 3-((3 -hydrobenzyl ) 黻 基) a 7-phenyl one (N-printed by the Central Standards Bureau of the Ministry of Economic Affairs Beigong Consumer Cooperative printed tributyl gas carbonyl Shen Shen) hexahydroxenon heterococoon 2-ketone (heteropolar ^ diastereomeric Base) 55% yield, mp 2 0 1-2 0 3 Ό 〇7 Η-NMR (δ, CDC 1 3): 1. 38 (s, 9Η), 1. 6 — 2 · 4 (successive multiple line, 6Η), 4. 05 (ΑΒ, Jab = 17, Δ „= 357, 2Η), 4. 5 — 4. 7 (m, 2Η), 6. 6-7. 8 (m, 1 1 Η) 〇IR (cm-, KBr): 1719, 1 6 8 0, 1 6 2 5 (C = 0) MS (%): 471 ( 14, parent), 415 (47), 3 4 5 (5 2), 2 8 9 (1 0 0), 127 (51), 83 (45), 55 (39) 0 analysis calculation C23H3〇N3〇4C1 : C, 63. 62; Η, 6.41; N, 8.90. Experiment: C, 63.74; H, 6.49; N, 8.62. Fen Shi Example 1 53— (3—Tian Rong, a urea), a 7—Jumou_ (Ν— 三 丁 气 撖 某 申 某), a six argon xenon hetero-H 2-ketone Gengli structure) 44% yield, mp 1 8 1-1 8 3 1C 〇 (please read the precautions on the back first and then this page) This paper scale is applicable to China National Broadcasting Standard (CNS) A 4 specifications (210 X 297 mm) -57 A6 B6 Printed by the Employees ’Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (55) 'H-NMR (δ, CDCla): 1.38 (s, 9H), 1. 6 — 2. 4 ( Continuous multiple lines, 6H), 2. 24 (s, 3 Η), 4. Ο 1 (A Β, J ΛΒ = 1 7, Δ, = 381, 2Η), 4. 5-4. 6 (m, 1Η ), 4. 62 (t, J = 7, 1 Η), 6. 57 (m, 1 Η), 6.76 (m, 1 Η), 7. 0-7. 5 (m, 9 Η) Ο IR (cm ·, KBr): 1721, 1680, 1 6 3 6 (C = 0) ○ Analysis and calculation C26H33N30 · 0.25H 2〇: C, 68. 47; H, 7.40; N, 9.21. Experiment: C, 68. 71; Η, 7. 4 7; Ν, 9. 22. Example 1 6 3-((3-argonyl urea) urea)-7-stupid one (N_ third butyl argon carbonyl a methyl)-a six argon argon heteroyl-2 Enantiomer) 44% yield, mp 169-170¾. 7H-NMR (3, CDCla): 1. 38 (s, 9Η), 1. 6-2. 4 (connected multi-line, 6Η), 3. 71 (s, 3 Η), 4. 0 2 (Α Β, J λΒ = 1 7, Δ, = 375, 2Η), 4.5-4. 7 (m, 2Η), 6.47 (m, 1Η), 6.50 (m, 1Η), 6.81 (m , LH), 7.0-7.6 (m, 8H) (please read the precautions on the back before filling in this page) This paper is also applicable to the standard ® standard (CNS> A 4 specifications (210 X 297 mm> -58 Α6 V. Description of the invention (56) IR (C m -1 t K Β Γ): 1 7 2 7, 1 6 2 8 (C = 0) 〇Analysis and calculation of C 2βΗ 3 3 Ν 3 0 5: C » 6 6. 7 9 • t Η, 7. 1 1; N »8. 9 9. Experiment • • C» 6 6 • 5 9; Η, 7. 1 2; Ν 9 8.9 9 2 ο Fen Shi Example 1 7 3-(ί 3-A Benzene poor) M group) -7-phenyl- (Ν- (please read the precautions on 3 sides before filling this page)

The third consumer of the Central Bureau of Standards of the Ministry of Economic Affairs has printed the third butyl argon carbonyl) a six-gas xenon complex 2 (lower polar diastereomeric structure) 39% yield, mp 180-9. π. ^ -NMR (δ, CDCla): 1.27 (s, 9H), 1 · 6 — 2. 4 (continuous multiline, 6H), 3. 69 (s, 3 Η), 3. 57 (AB, J λΒ = 1 7, Λ, = 226, 2Η), 5. 01 (m, 1 Η), 5. 08 (m, 1 Η), 6.45 (m, 1 Η), 6.8 (m, 2H), 7.0 -7.6 (m, 8H) 〇IR (cm-, KBr): 1741, 1640, 1 605 (C = 0) 〇 MS (96): 467 (11, parent), 159 (32), 123 ( 1〇0), 117 (25) 〇 analysis and calculation of CwH33N3〇5 · 0.5H2〇: C, 65. 5 3; H, 7.19; N, 8.82. Experiments: C, 6 5. 4 4; Η, 6. 9 5 2; Ν, 8. 84. Bookbinding Λ The standard of this paper is the General Chinese Standards (CNS) A 4 specifications (210 X 297 ;;) -59 Ministry of Economic Affairs Central Standards Bureau employee consumer cooperation du printing A6 B6-V. Description of invention (57) 1 8 3 —— ((3 鰱 Benzhua) Urea hua) 7 7 benzoxanthone (Ν 第 T oxycarbonyl 荜 菜菜 华) »-radon radon mixed leather 2 m (lower handle diastereomer M . Structure) 1 9% fish rate t foam Ο 1 Η--NMR (δ, CDC 1 3) • »1 • 2 6 (S t 9 Η)> 1. 6 — 2 * 4 (intertwined multi-line »6 Η) > 3 • 5 1 (AB t JAB = 1 7 9 Δ V = 1 9 5 9 2 Η) 9 5 ♦ 0 0 (m > 1 Η) 9 5 • 0 8 (mt 1 Η) t 6 ♦ 8 —1 7 ♦ 4 (mt 9 Η) »7 • 9 8 (width st 1 Η) t 8 • 1 3 (width s 9 1 H) Ο 13 Η -N Μ R (δ» CDC 1 3 ) • _ 2 7.] L, 2 7 • 8, 3 1 • 1 t 3 1 • 8 t 4 6 • 8 t 5 2 • 7 t 6 0 • 5, 6 1 • 9 1 8 1 «7 9 1 1 7 • 2 ♦ 1 1 7 • 3, 1 1 7 • 4 t 1 1 9 • 4 t 1 2 2 «5 9 1 2 2 • 8, 1 2 8 • 7 f 1 2 9 • 1 t 1 2 9 • 7 9 9 1 2 9. 8 2, 134.4, 134.5, 1 3 8. 1, ο4 1-

ο • 3 5 1X, 5 ο 4 1X

2 • 5 5 1X 〇 2

r B .K 〇5 ») 7 7 0 :) 1 m-) 5, cc% 3 / fv / f \ / l \ .R 8 s 9 8 I 9 M 2 6 5 1 1 1 I 3 ((7 12 714 代 亲 ο 9 2 6 1i 0 2 2 2 / IV / 1 \ 5 7 4 1 3 1 (please read the precautions on the back before filling this page) -installation. Order_ This paper size is applicable to Chinese national standards (CNS) A4 specifications (210 X 297 mm) -60 A6 91 printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs: 19C1_B6_ V. Description of inventions (58), 83 (41). HRMS calculation C25HwN3〇4C 1: 471 . 19411. Experiment: 471. 19455. Fen case 1 9 3-(3-a certain urea) a 7-a certain (N-2-adamantane) americium a) a six argon 42% yield of leather 2-ketone, mp 120-1301C. 2H-NMR (5, CDC13): 1.4-2.4 (interlaced multi-line, 20H), 2. 23 (s, 3H), 3.71 (AB, J ab = 1 7, Δ, = 213, 2H), 4. 7 5 (m, 1 H), 5.0 4 (m, 1 H), 5.1 (m, 1 H), 6. 75 (m , 2 H), 7. 0-7. 6 (m, 9 H). IR (cm'1, KB r): 1750, 1650 (C = 0) MS (96): 529 (8, parent) , 159 (46), 135 (49), 133 (47), 117 (31), 107 (1 0 0), 85 (3 9), 83 (3 9) Calculate C32H39N3〇4 * 0.5H2〇: C, 71.35; Η, 7. 48; Ν, 7. 80. Experiment: C, 71.7 2; Η, 7. 3 3; Ν, 7. 80. Fen Shi Example 2 0 (Please read the precautions on the back before filling in this page) The paper size is in accordance with the specifications of China Sleepy Family Standard (CNS) A 4 (210 X 297 mm) -61 A6 ^-V. Description of invention (59 ) 3- (3-tolyl ureido) a 7-phenyl one (N-(L-all the 丨 alkyl) Xi Shen Shen) a six argon gas seal 2- 2- ketone 3% yield, foam. H-NMR (5, CDC13): 1.4-2.4 (continuous multiple lines, 20H), 2. 26 (s, 3H), 3. 57 (AB, Jn = 17, = 250, 2H), 5.0 2 (m, 1 Η), 5.1 (m, 1 Η), 6.7 -6.8 (m, 2H), 7.1-7.4 (m, 9H) 〇IR (cm'1, KB r): 1745 , 1 6 5 0 (C = 0) MS (%): 529 (14, parent), 378 (60), 159 (78), 135 (1 0 0), 107 (60 HRMS calculation C32H3sN3〇4 : 529. 29403. Experiment: 529.2902. Note

I i Ministry of Economic Affairs Central Bureau of Standards and Staff Cooperative Printing Duo Cao Shi Example 2 1 3 — (3-methyl ureido) 7 — stupid 1 (N — (1 — adamantane) carbonylamide ) A six-argon xenon mixed leather 2_ 28% yield, mp 145-1541C. ^ H-NMR (5, CDC13): 1.4-2.4 (intertwined multi-line, 2〇H), 2. 245 (s, 3H), 3. 50 (AB, J λ B = 1 G, Δ, = 174 , 2H), 5. 03 (m, 1 H), 5. 1 (m, 1 H), 5. 26 This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -62 V 、 Description of the invention (60)

S Η), 6. 7 — 6.8 (m, 2H), 7. 1-7.7 (m, 9 Η) 0 IR (cm · 1, KBr): 1645 (extremely wide) (C = 0) 〇MS (96): 528 (< 1, parent), 203 (36), 133 (1 0 0), 132 (3 0), 1 17 (4 4), 107 (61), 104 (31) . Analysis calculation C32H4〇N4〇3 0.5H2〇: C,

71. 48; H, 7. 69; N, 10. 42. Experiments: C, 71.33.7; H, 7.80; N, 10.29. Example 2 2 4 A stupid-fi-methyl-1 · 2 · 3 · 4-tetrahydrorazine-1 1 was prepared according to the method of JACS, 69, 74 (1947) (shown in diagram 4): A . 3 — He Yi Yi (4 · Yi Chang Mou. Ji Yi (3 — Jia Mou Rong Mou)) 1 Ding Yi 3 — Central Bureau of Standards of the Ministry of Economic Affairs®: A6 B6 printed by the industrial and consumer cooperative (please first MfRJe Note on the page and write this page again) Add a 250m5 round bottom flask equipped with a condenser and N2 inlet to add lOOmi third butanol, 12.57g (112 ·· 〇1) potassium third butoxide, 20g (102 mmol) 3-methyl benzophenone, and 21. 31g (122 «mol) diethyl succinate. The reaction was refluxed for 14 hours, cooled, acidified with HCI ?, and then distributed between water and ether. This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) Printed A6 ^-V. Description of the invention (61). The organic layer was washed with 1N hydrogenated sodium aqueous solution, then acidified and extracted into ether. The organic layer was dried and concentrated into an oil for direct use. B. (4 — Rongmou.4 one (3 — A certain Rongmou) a butan-3-enoic acid oil at 60m) 2 acetic acid, 60ιηβ 48% mandarin bromate, and 5 Οιηβ additional acetic acid solution heated to reflux 1 4 hours to dissolve it. The brown oil separated by cooling alone was dissolved in ethyl acetate, washed with water, and then washed with 2% aqueous sodium hydroxide solution. The basic aqueous phase was acidified, extracted into ethyl acetate, dried, and concentrated. The product is a mixture of olefin isomers, NMR: JH-NMR (5, CDC13): 2.27 and 2.29 (s, 3H), 3.19 (m, 2H), 6. 1 8 (t, J = 7, 1 Η), 6.8-7.4 (m, 9 Η) 〇C. (4-Zhu Mou · 4-(3-methylphenyl) monobutyric acid above oil (25.7 g) in ethyl acetate to 1. 10% of the 25s 10% Shuo rake hydrogenated under 30p.si hydrogen for 2 hours. Filter through Celite and shrink, then chromatography on silica gel, using methanol / dichloromethane as eluent to produce oil, which is produced by heptane Alkane crystals, 4.70s (18%), M.P. 96-100C. 'H-NMR (δ, CDCIj): 2.35 (s, 3 Η), 2. 2-2.3 (m, 4 Η) , 3. 95 (t, < please read the notes on the back before filling in this page)-Binding · Order. This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -64 B6

m ^ c, 1- V. Description of the invention (62) J = 7 »1 Η) * 7 * 0-7 • 4 (m, 9 H) 〇i 3 C -N MR (δ t CD c 1 3): 2: 1. 6, 3 0 • 3 t 3 2 • 6 * 5 0 • 4 9 1 2 4. 8 f 1 2 6 • 5 f 1 2 7 • 3 * 1 2 7 • 9, 1 2 8 • 5 , 1 2 8 »6 t 1 3 8 • 2 $ 1 4 3 • 9, 1 4 4 • 2, 1 8 0 • 3 o IR (C m -1 1 KB r) • 1 7 2 0 (C = 0 ) O Μ S (%) • Qin 2 5 4 (parent f 2 3), 1 8 2 (1 0 0) 9 1 6 5 (2 3) 9 3 2 (3 6) 9 2 8 (1 0 0 ) 0 Analyze and calculate C i 7 HI 8 0 2: c 8 0. 2 8, H 7 • 1 3 0 experiment • C 8 0 • 5 4 f H 7 • 0 5 o D • 4 Benz Hua 6 Jia Hua 1 • 2 • 4 Siqifang—1 — BpI (Please read the notes on the back before writing this page) The Central Standards Bureau of the Ministry of Economic Affairs prints 25〇111 with a condenser and N2 inlet. 2 round bottom To the flask, add 8.2g (32.3 methane weight 〇1) (4-phenyl, 4_ (3-methylphenyl)) butyric acid, 54mi toluene, and 4.6g (38.64 mmol) thionyl chloride . The reaction was refluxed for 1 hour, cooled and concentrated. This oil was dissolved in 15mP disulfide master, and added dropwise to 29.98g (225 mB〇l) aluminum chloride slurry in 50m) 2 disulfide which had been cooled to 0¾. The reaction was left for 16 hours, poured onto ice, and distributed between water and ethyl acetate. The organic phase was washed with water, aqueous sodium hydrogenate, and water, then dried and evaporated. The oil is chromatographed on silica gel and uses hexane / ethyl acetate. The paper is again applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm). It is an eluent that produces oil, 4.03g (53%). &Quot; H-NMR (δ, CDCla): 2.28 (s,

3 Η) 9 2 • 2 one 2 • 7 (mt 4 H), 4 • 2 4 (m, 1 Η) »6 • 8 one 7« 4 (m »7 H), 8 • 0 2 (t, J = 7 9 1 H) 0 i 3 c —— NMR (δ tc D c 1 3) • 2] L. 8, 3 1 • 9 t 3 6 * 4 »3 6 • 5 f 4 5. 2 9 1 2 6 8, 1 2 8 • 1 t 1 2 8 • 5, 1 2 8 ♦ 6 • 1 2 9 • 9 f 1 3 0 • 6 »1 4 3 • 8, 1 4 4 • 5 $ 1 4 6 • 2 t 1 9 7 • 8 〇IR (cm -1 * KB r) ♦ 1 6 8 0 (C = 0) OMS (%) * 2 3 6 (parent »9 6) t 2 0 8 (9 2) t 1 9 4 (4 2) »1 6 6 (4 3) OE · 4 -Phenyl-R-Methyl- 1. 2. 3. 4 — ^ Qi Xi (please read the notes on the back before writing This page > i Pack · Order · ^ 乂 · Ministry of Economic Affairs Central Standards Bureau R Industrial and Consumer Cooperatives Cooperative Department-1 _ Surrounded by a condenser and N2 inlet 1 251115 round bottom flask add 4. 3g (18. 29 mmol) 4 — Phenyl-6-methyl-1,2,3,4-tetrahydro-any 1-one), 46mi? methanol, 2.95 g (29.26 mn〇l) triethylamine, and 2. 02g (29.26 mm〇l) hydroxylamine hydrochloride. The reaction was stirred at room temperature for 3 days, evaporated, distributed between ethyl acetate and water, and the aqueous layer was extracted with fresh ethyl acetate. The combined organic layer was dried with sodium sulfate and evaporated to an oil, 4.57g (100%). This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm > -66 21 ο Ο-Γι A6 B6 Printed by R Industrial and Consumer Cooperatives, Central Bureau of Standards, Ministry of Economic Affairs V. Invention Instructions (64) 2 Η --Ν Μ R (d, CDC 1 ί 3) ♦ 2 1 one 2 • 3 (m $ 2 Η) t 2 • 2 8 (S »3 Η) f 2 • 8 one 3 • 0 (m $ 2 Η ) f 4 • 1 7 (mf 1 Η) t 6 • 8-7 • 4 (mf 7 Η) 9 7 • 9 5 (d »J = 7» 1 Η) 〇I 3 C-Ν MR (d 9 CDC 1 3): 2] L. 1, 2 1 ♦ 4 »2 9 • 6 > 4 5 • 0 t 1 2 6 • 5 > 1 2 8 • 0 f 1 2 8 • 1 9 1 2 8 ♦ 5 f 1 2 9 • 2 9 1 2 9 «9 t 1 3 9 • 7 1 4 1 4 • 1 4 4 • 0 1 5 5 ♦ 3 Ο IR (C m -1 9 KB Γ) • • 1 6 1 0 (C = Ν) 〇MS (%) • • 2 5 1 (parent t 9 4) t 2 3 4 (3 2), 1 5 6 (1 7) 1 9 1 (1 7) ο HR Μ s calculation C 1 7 Η 1 7 Ν 0 • 2 5 1 • 1 3 1 0 0 experiment • • 2 5 1 • 1 3 0 2 2 0 F • 5 Phenol 7 甲 荸 ρ, • 3 • 4 Lusi gas 1 η (1) benzene ψ 氤 杂 单 ρ> Ketone with Ν 2 2 5 0 m inlet 9. Add to the bottom flask 4 5 g (1 8 • 3 mmol) 4 — benzene Hexa-6 monomethyl — 1 9 2 $ 3 • 4 one tetrahydro certain ketone oxime and 5 9 • 4 5 g polyphosphoric acid Ο mixture in 1 3 〇 It was heated in an oil bath for 2 5 minutes, and then poured Place on ice and mix well. The mixture was extracted with ethyl acetate, the organic layer was washed with water and brine • dried over sodium sulfate, and evaporated. The residue is chromatographed on silica gel, using hexane / ethyl acetate as the eluent to produce oil, 2. 2〇g (49%), which can be (please read the precautions on the back before filling this page) L .. Binding · Ordering. R4. This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 public potentiometers) — 67 丄 _B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of invention (65) Crystallization of methane and isopropyl ether produces solid tm P 1 6 9-1 7 3 V 〇2 Η--NMR (δ, CDC 1 3) • * 2 • 1 6 (S, 3 Η) 9 2 • 4 — 2 • 6 (mf 4 Η) t 4 • 4 0 (m »1 Η) 9 6 • 6 and 7 • 0 — 7 • 4 (mt 8 Η) * 9 • 1 5 (bst 1 Η) 0 1 3 C — N Μ R (δ »c D c 1 3) • • 2 1 •] L, 3 2 • 9 9 3 3 • 9 9 4 5 • 0 9 1 2 1 • 9» 1 2 7 «〇 * 1 2 7 * 9 > 1 2 8 • 6 * 1 2 9 • 0 1 2 9 * 1 1 3 5 • 0 f 1 3 5 • 2 9 1 3 6 • 5 t 1 4 1 • 2 9 1 7 5 • 8 Ο IR (cm -1 t κ Β r) • • 1 6 8 0 (C = 0) O Μ S (%) • • 2 5 2 (parent + 1 9 1 0 0) f 1 9 6 (1 0) t 1 4 7 (1 0), 1 3 5 (1 4) 9 1 1 9 (1 3) »1 0 3 (1 2) ο Analysis and calculation of C 17 Η 17 Ν 0 • c 8 1 • 2 4 t H 6 • 8 2 N 5 • 5 7 Ο Experiment • • C 8 1 • 0 4 »H 6 • 6 9» N 5 • 4 7 ο The rest of the synthesis is the same as in Example 1 0 G 3 carries 5 Phenol 7 Jiahua 2 • 3 «4« 5 four gas 1 H (1) Phenanthrene 2 ketone M P 2 0 5 2 1 1 V »6 2% yield o JH-NMR (δ, CDCla): 2. 13 (s, (please read the precautions on the back before filling in this page) This paper size is applicable to the troubled countries Standard (CNS) A4 specifications (210 X 297 mm) -68 A6 B6 V. Description of invention (66) Printed by the Employees Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 3 Η) 9 2 • 8 3 (m »1 Η) 9 3 • 0 9 (m »1 H) > 4 • 4 2 (m 9 1 Η) t 4 • 6 2 (m» 1 Η) 9 6 • 6 and 7 • 0 a 7 • 4 (mt 8 H) 9 8 • 9 9 (bs »1 Η) 〇1 3 C — NMR (δ 9 c DC 1 3) • • 2 1 • 1 f 4 5 ♦ 0 t 4 6 ♦ 1 t 4 7 • 3 »1 2 2 • 5» 1 2 7 • 4 »1 2 8 * 3 9 1 2 8 • 6 > 1 2 8 • 8 »1 2 8 • 9 > 1 3 3« 5 f 1 3 3 • 6 > 1 3 5 • 8 > 1 3 6 • 4 1 3 9 • 3 > 1 6 9 • 3 Ο IR (cm -1 9 Κ Β Γ) • • 1 6 7 8 (C = 0) 〇Μ S (%) 3 3 0/3 3 2 (Parent > B Γ 7 9 / B Γ 8 1 t 1 0 〇 / 9 8) t 2 5 1 (2 6) f 1 3 7 (3 2) 9 1 1 9 (3 2) t 8 5 (2 7) 〇Analysis calculation C 2 7 Η 1 6 Ν 0 B r # C 6 1 ♦ 8 3 f H 4 ♦ 8 8 N 4 * 2 4 O Experiment C 6 1 • 7 9 9 H 4 • 5 7 > N 4 • 0 9 0 Η • N 2nd Dinghua 2 3 m 2 Oxygen 5 Benhua 7 Jiahua 2 «3 • 4« 5 Four gas 1 Η (1) benzene diazepine extraction 1 Hua 1 amide amine M P • 1 2 9 1 3 3 V t 9 3% yield Ο i Η--NMR (δ, CDC: 1 3) • 1 • 3 3 (s »9 Η) > 2 • 1 4 (S» 3 Η) t 2 • 8 3 (m 1 H) 9 3 • 〇1 (m 1 Η) 9 4 • 3 1 4 5 (m 9 2 H) (Be sure to read the precautions on the back before filling out this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 Specifications (210 X 297 mm) -69 glu90i A6 B6 Printed by the Central Standards Bureau of the Ministry of Economic Affairs, the 8 Industrial and Consumer Cooperatives V. Invention Instructions (67) 9 4 • 5 9 (mf 1 Η) 9 4 • 6 6 (mt 1 H) f 6 • 1 4 (bs 9 1 Η) 9 6 • 4 8 (bst 1 H) t 7 • 0 a 7 • 4 (m 9 8 Η) Ο I 3 C — NMR (δ 9 CDC 1 3) <: 2] • 2, 2 8 «7% 4 3 • 9 > 4 5 ♦ 7» 4 7 • 3 > 5 1 • 5, 5 4 • 8 9 1 2 3 • 0 »1 2 7 • 3 »1 2 8 • 3 f 1 2 8 • 7 $ 1 2 8 * 8 9 1 2 8 • 9 t 1 2 9 • 0 9 1 3 7 • 4 9 1 3 7 • 5 9 1 3 8 • 4 1 1 3 9 9 1 * 1 6 7 • 1 t 1 6 8 • 2 Ο IR (cm -1 9 κ Β Γ) • «1 6 6 2 (C = 0) 〇Μ S (%) • 4 4 3 / 4 4 5 (Parent t B r 7 9 / B Γ 8 1 f 9 0/9 2) t 3 7 0/3 7 2 (B r 7 9 / B Γ 8 1 t 1 0 0/9 8) 9 2 9 〇 (5 〇) f 2 6 2 (4 5) 9 1 3 4 (6 5) Ο Analytical calculation C 2 3 H 2 7 Ν 2 0 2 Β Γ 1/3 H 2 0: C 6 1 • 4 7 t H 6 • 2 1 9 Ν 6 • 1 2 0 Experiment: C 6 1 • 2 0 9 H 6 * 1 2 > Ν 5 • 9 6 0 IN Di Dinghua 2 Γ 3 Lip Nitrogen 2 Oxygen 5-Benhua 7 Jiahua 2 «3« 4 «5 Four Radon 1 H (1) Benzene and radon leather 1 _ Hua] acetamide foam, a mixture of diastereomers, 81% yield. ^ H-NMR (δ, CDC13): 1.27, 1. 32 (s's, 9 Η), 2. 12, 2, 37 (s 1 s (please read the precautions on the back before writing this page) 丨 Pack- Order · This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -70 A6 _B6 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Invention Instructions (68) 9 3 Η) t 2 ♦ 7 8 (mf 1 H) t 2 • 9 5 (m 9 1 H) > 2 • 9 8 (ABQ f J Λ B = 1.5, Δ, = 2 7 9, part) 2 Η) f 3 • 8 2 t 3 • 9 6 • 4 • 0 6 »and 4 • 6 4 (multi-wire parameter 2 H) 9 4 parameter 3 5 (s $ remaining 2 H) t 6 • 1 7 (bs» 1 H) »6 • 4 5 (bst 1 H) t 7 • 0 — 7 • 4 (mf 8 H) 〇13 C — NMR (δ 9 CD c 1 3) • • 2] L. 0, 2 1 • 2 9 2 8 • 6 t 2 8 • 7 f 3 5 • 5 9 3 9 • 8 »4 1 • 9 9 4 3 • 7 9 5 1 • 3 9 5 1 • 5 9 5 4 • 6 5 8 • 3 9 5 9 • 〇 9 6 〇 • 4 t 1 2 3 • 0 »1 2 5 • 6 9 1 2 6 • 1 > 1 2 6 • 5» 1 2 7 • 3 > 1 2 7 • 3 3 f 1 2 7 • 4 t 1 2 8 • 2 9 1 2 8 • 3 »1 2 8« 4 * 1 2 8 • 5 f 1 2 8 • 6 1 2 8 • 6 5 9 1 2 8 «7 t 1 2 8 • 8 f 1 2 8 • 9 $ 1 2 9 • 5 8 9 1 2 9 «6 4 9 1 3 0 • 9 9 1 3 7 • 2 9 1 3 7 • 6 $ 1 3 7 • 7 t 1 3 8 • 5 t 1 3 9 • 4 9 1 4 1 • 1 »1 6 7 • 1 $ 1 6 7 * 9 t 1 6 9 • 9 t 1 7 0 • 4 0 IR (cm -1 f KB Γ) • 2 0 9 8 (N 3) f 1 6 6 0 (C = 0) o M S (%) • 4 0 6 (parent + 1 t 7 4) 9 3 8 0 (4 3) 9 3 4 7 (4 1), 3 3 3 (1 〇0) 9 2 4 9 (4 5) f 2 3 4 (6 2) t 2 2 2 (7 7) > 2 2 0 (7 4) > 2 0 8 (7 9) 9 1 4 4 ( 5 1) 9 1 3 2 (41), 105 (47), 91 (90). (Please read the precautions on the back before filling in this page) This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm> -71, A6 fj * · V. Description of the invention (69) Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs Η Ｍ Ｍ Ｓ ＭＡＭＭ 1 6 5 ο Experiment • 4 0 5 .2 1 6 2 2 0 J Ν Second Ding Hua 2 r 3 amine oxalic acid 5 benzene chrysanthemum 7 Jiahua-1 3 4 5 tetra radon 1 Η (1) benzyl hydride extraction 1-Hua Ί acetic acid amine M • Ρ • 10 0 1 1 0 t: f diastereoisomerism 9 2 9% yield Ο 1 Η--Ν Μ R (δ, CDC 1 3) • • 1 * 2 4 t 1 • 3 1 (S • S, 9 Η) «2.] L] L, 2. 3 5 (s S t 3 Η) 9 2 .6 2 (b S 9 2 H) 9 2 • 6-2 • 8 (mt 2 Η) > 3. 2 — 3 • 4 (mt 2 Η) > 4 • 0 — 4 * 5 (m »4 Η) t 6 * 0 9 (bs 9 1 Η) t 6 • 4 (b S% 1 Η), 7 • 〇— 7 • 4 (m 9 8 Η ) Ο IR (C m -2 * Κ B r) • 1 6 6 0 (C = 0) Ο Μ S (96): 3 7 9 (parent 1 2) »3 3 6 (1 7) ί 2 3 5 (1 6) 9 2 0 2 (2 2) f 3 2 (3 5) 9 2 8 (1 0 ◦) ο Η R Μ S calculation c 2 3 H 2 9 N 3 0 2: 3 7 9 • 2 2 6 0 Ο Experiment 3 7 9 .2 2 8 4 8 〇 Analysis and calculation C 23 Η 2 9 N 3 0 2 2/3 Η 2 0: C 7 0 • 5 6 t Η 7 〇 • 5 6 t H 7 • 8 1 »Ν 1 〇 • 7 3 Ο experiment • C 7 0 • 6 4 f Η 7 • 4 7» Ν 1 0 • 0 4 (-0 • 6 9) 〇 (please read the precautions on the back first Write this page) This paper scale is applicable to China National Standards (CNS) Grade 4 (210 X 297 mm)

AIBI V. Description of the invention (70) K. N — 玮 三 丁某 2-Γ3 — (3 __—- L..3 — Toluene) gland) one 2 — atmosphere one 5 — cage one 7 — Shenhua_ 2_1—2_I—4_I_ 5 —Four gas one: LH- (1) ju # arga hetero M-1 monoyl_1 oxalyl acetate to obtain a mixture of diastereomers, one of which is precipitated by the anti-mix Polarity); the other is purified by means of analysis (lower polarity). The more polar isomer, M.P. 280-283t :, 45.5% yield. 'H-NMR (δ, CDC13): 1. 30 (s, 9 Η), 2. 11 (s, 3 Η), 2. 22 (s, 3 Η), 2. 8-3. 2 (m, 2Η), 3. 90 (m, 1 Η), 4.34 (ΑΒ,, Jxs = 16, A ν = 59, 2Η), 4.62 (m, 1Η), 6.4-6.8 (multiple Line, 3H), 7.0-7.4 (m, 12H) o IR (cm-i, KBr): 1640 wide (C = 0). FAB MS (96): 513 (parent +1, 7), 3 8 0 (9 8), 3 0 7 (5 3) · 155 (51), 119 (10 0) Printed by the consumer cooperative (please read the precautions on the back and then «write each page> HRMS calculation ChH mN 4〇3: 512. 27511. Experiment: 512. 27528.

Analysis calculation · 2 / 3H20: C 7 0.97, H 7.17, N 10.68. Experiments: C 70 · 80, H, 6.71 (-0. 46), N 10. 3 9 〇 This paper scale is applicable to China's β standard (CNS> A 4 specifications (210 X 297 g ** -73 A6 B6 5 2. Description of the invention (71) (Please read the precautions on the back before writing this page) The less polar isomer, M.P. 130-1351C, 42% yield. 'H-NMR (d, CDCla ): 1. 26 (s, 9 Η printed by the Industrial and Commercial Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs) t 2 • 2 1 (st 3 H) »2 • 3 8 (st 3 H)» 2 • 7 7 (m » 1 H) »3 • 0 1 (m 9 1 H) t 3 • 2 2 (ABQ 9 JAB = 1 6 $ △ V = 2 8 7 t 2 H)» 4 • 1 5 (m &gt; 1 H), 4 • 6 0 (mt 1 H) »5 • 8 9 (bs 1 H) 9 6 • 5 — 7 • 3 (m 9 1 3 H) &gt; 7 • 6 7 (bsf 1 H) 〇13 CNMR (d »CDC 1 3) 4 &lt;: 2] L. 0, 2 1 • 4» 2 8 • 6 f 3 7 • 1 t 4 4 • 4 t 5 0 • 2 t 5 1 • 6 9 5 3 • 6 f 1 1 6 • 7 9 1 2 3 • 4 9 1 2 3 • 5 f 1 2 6 • 3 f 1 2 6 • 4 9 1 2 8 ♦ 3 t 1 2 8 • 6 »1 2 9 • 4 &gt; 1 3 1 • 3 9 &gt; 1 3 1 • 4 3 &gt; 1 3 7 • 7 »1 3 7 • 9 9 1 3 8 • 5» 1 3 8 • 6 1 3 9 • 1 9 1 4 1 • 9 9 1 5 5 • 4 9 1 6 7 • 6 t 1 7 3 • 0 0 IR (C m -2 9 KB Γ) • 1 6 4 0 width (C = 0) 〇FABMS (96): 5 1 3 (parent + 1, 7 8) 9 4 4 0 (9 8) 3 8 0 (4 6) »3 0 5 (4 4) f 2 5 1 (7 7)» 2 3 4 (9 3) t 2 2 2 (6 7) 1 2 2 0 (4 5) * 2 0 8 (1 0 0), 1 4 4 (4 4) 1 0 7 (5 4) 〇HRMS calculation C3iH3 <; N4〇3: 5 1 2. 2754 1 This paper scale is applicable to the national standard (CNS) A 4 specifications (210 X 297 mm> -74 A6 B6 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Invention Instructions (72). Experiment: 512. 28240. Analysis and calculation CnH36N4〇3 · l / 2H2〇: C 7 1. 5 8, Η 7. 15, N 10. 74. Experiment: C 71.55, Η 7.10.Ν 10.33 (-0.41). Fen Shi Example 2 3 Ν — 箆 三 丁某 2 — f3 — (3— (3— 氣 朱某) Μ 基) 一 2 — 气 一 5-Stupid certain 7 — A certain 2. 3. 4. 5 — Siqi ~~ 1Η — (1) Benbenqiza leather-1 monoyl] acetamide acetic acid is a mixture of diastereomers prepared from the target compound of Example 2 2 J, one of which is precipitated by the reaction mixture (polar The higher) · The other is purified by chromatography (lower polarity). The more polar isomer, M.P. 282-285¾, 38% yield. 2H-NMR (δ, CDC13): 1.28 (s, 9 Η), 2. 10 (s, 3 Η), 2. 8-3. 2 (m, 2 Η), 3. 9 0 (m, 1H) , 4.32 (AB ,, J a B = 1 6, Δ, = 52, 2H), 4. 57 (m, 1H), 6.42 (bs, 1 H), 6. 6-7.4 (m, 1 4 H) 〇IR (cm ·, KBr): 1640 wide (C = 0) 0 FAB MS (96): 533/535 (parent +1, C135 / C137, 9/4), 380 (52), 307 / (please Read the precautions on the back first and then fill out this page) This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -75 A6 B6 V. Description of invention (73) 3 0 9 (29/11) , 155 (7 0), 135 (46), 119 (1 0 0), 103 (6 8 〇 analysis calculation C3〇H33N4〇3C 1 ♦ 1 / 2Η2〇: C 6 6. 4 7, Η 6. 3 2 , Ν 10. 34. Experiments: C 6 6. 17, Η 6. 2 5, Ν 10.04. The less polar isomer, Μ Ρ. 155-165t :, 46% yield. (Please first Read the precautions on the back and then write this page) Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 2 Η--Ν Μ R (δ, CDC] 1 3) ♦ • 1 • 2 8 (st 9 Η) t 2 • 3 9 (st 3 H) »2 ♦ 8 a 3 • 0 (m 2 Η) t 3 • 2 8 (AB &lt; 1 t JAB = 1 6 »Δ V = 2 8» 2 Η) »4 • 1 1 (m 9 1 H) t 4 • 3 8 (m» 1) &gt; 5 • 8 3 (bs &gt; 1 H) t 6 • 6 — 7 • 2 (mt 1 2 Η) »7 • 5 7 (bs 1 H) &gt; 7 • 9 8 (bs 1 Η) ο 13 C — Ν Μ R (δ f CDC 1 3) K *: 2 ] L. 0, 2 8 • 7 9 3 6 • 8 »4 4 • 4 t 5 0 • 4 t 5 1 • 8 5 3 • 2 $ 1 1 6 • 9 9 1 2 2 Reference 1, 1 2 6 • 3 »1 2 6 • 5 &gt; 1 2 8 • 3 t 1 2 9 • 5 t 1 3 1 • 5» 1 3 4 «3 t 1 3 7 • 7 f 1 3 7 • 8 t 1 3 7 • 9 } 1 3 8 • 4 9 1 4 0 • 7 t 1 4 1 • 9 »1 5 5 • 1 &gt; 1 6 7 • 4 f 1 7 3 * 3 〇IR (cm -1, KB Γ) • 1 6 4 0 Width (C 0) FA Β Μ s (%) • 5 3 3/5 3 5 (Parent + 1 C \ 35 / C \ 37, 37/15), 460/462 (81 paper size for China National Standards (CNS) Grade A 4 (210 X 297 mm) -76 Printed by the Employees ’Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs Q ^ A6 ^ _B6_ V. Description of Invention (74) / 31), 3 8 0 (3 3) , 3 0 7 (6 1), 251 (61), 2 3 4 (1 0 0), 2 2 2 (6 2), 2 0 8 (9 9), 91 (51). Analysis and calculation of C wH 33N 4〇3C 1: C 6 7.5 9 8, H 6. 2 4, N 10. 51 . Experiment: C 6 7.50, H 6, 18, N 10.14. Fen Shi Example 2 4 N — third Ding 2 — “3 — (3 — (3 — A M Zhu) Urea) — 2 — argon — 5-phenyl — 7 — methyl — 2. 3.4. 5 One four argon one 1H-(1) Juxenoxenium leather one 1-yl] acetamide acetate The mixture of diastereomers prepared from the target compound of Example 2 2 J, one of which was precipitated by the reaction mixture (high Polar); The other is purified by chromatography (lower polarity). (Please read the precautions on the back before filling in this page) The more polar isomer t M. P. 2 8 3 — 2 8 6 V f 4 7% yield. 2 Η--NMR (δ, CDC 1 3) • 1 • 3 1 (sf 9 Η), 2. 11 (st 3 H), 2 • 8-3 • 2 (mt 2 Η), 3.7 (single peak t 3 H), 3 • 5 0 (m, 1 H) f 4 .2 9 (AB 9 »J Λ β = 15 t △ V = 1 3 8> 2 H) s 4. 4 6 (m, 1 H), 6. 4 — 7 • 4 (multiple males • 1 5 Η) Ο IR (C m &quot; 2, KB r): 1 6 4 0 width (c 0) o FAB MS (96): 529 (Parent +1, 7), the paper size is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -77 A6 B6 V. Description of the invention (75) Printed by the Employees Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 3 8 0 (1 0 0) * 3 0 7 (9 2) »2 5 1 (4 7) 9 2 0 8 (4 2) o Analysis and calculation c 3 1 H 3 6 N 4 0 4 ♦ 1/2 H 2 0:: C 6 9 • 2 5 »H 6 • 9 4 9 N 1 0 • 4 2 o Experiment • • C 6 9 • 2 2 f H 9 6 • 5 9 f N 1 0 • 2 4 o The lower polar isomer f M • P • 1 2 0 — 1 2 5 V &gt; Yield 3 7% 〇Μ--NMR (δ, CDC 1 3) 1 • 2 5 (S t 9 Η) t 2 • 3 8 (s &gt; 3 H) t 2 • 7 9 (mt 1 H) 9 3% 0 3 (mt 1 H) »3 • 2 5 (AB &lt; 1 negative JAB = 1 6 9 Δ ν η = 2 6 0 9 2 H) f 3 • 6 8 (S $ 3 H) »4 • 1 7 (mt 1 H) f 4 • 6 2 ( mt 1 H) 9 5 • 8 4 (bst 1 H) t 6 • 5-7 • 3 (mf 1 3 H) »7 • 8 0 (b S f 1 H) 〇13 C — NMR (δ 9 CD c 1 3) 4 •: 2 1 L. 0, 2 8 • 6 t 3 7 • 2 9 4 4 • 3 »5 0 • 1» 5 1 • 6 9 5 3 • 6 9 5 5 • 1 t 1 0 4 • 7 1 0 8 • 8 9 1 1 1 • 5 t 1 2 4 • 5 f 1 2 6 • 3 »1 2 6 • 4 9 1 2 8 • 3 f 1 2 9 • 3 * 1 2 9 • 4» 1 3 7 • 7 * 1 3 8 • 0 $ 1 3 8 • 5, 1 4 0 • 6 1 4 1 • 9 9 1 5 5 * 2 »1 6 0 * 1 t 1 6 7 • 5 t 1 7 2« 9 〇IR ( cm -1 »KB Γ) * • 1 6 4 0 wide (c = 0) 〇FA Β M s (%) • • 5 2 9 (parent + 1 f 8 3), (please read the notes on the back first Matters are written on this page again) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -78 A6 B6 V. Description of the invention (76) 456 (1 0 0), 3 8 0 (4 4), 307 (70), 251 (52), 234 (67), 208 (65). Analytical calculation C: »iH3eN4〇4 · Ι / 3Η2Ο: C 6 8.8, Η 6.96, N 10. 36. Experiment: C 68.94, Η 6.67, N 10.00. Example 2 5 N—T-Butyl 2— [3— (3— (3-Shenbenyl) ureido J-2—Flame_5— (3-Venylphenyl) —2. · ?. d ·. R- 四 气 一 1 Η-(1) Ju and 氤 璤 璪 一 1 a certain Ίacetic acid tyramine A. 4 a stupid one 6-gas one 1 · 2 · 4-four arginine in toluene Treat (4-phenyl, 4- (3-gas phenyl)) butyric acid with sulfurous sulfide gas (preparation method is similar to that of Example 4 4-phenyl, 4- (3-methylphenyl) butyric acid), then Cyclization in aluminum disulfide with chlorinated aluminum produces the desired 4- (3-aminophenyl) -1,2,3,4-tetrahydrobenzyl-1 ketone and isomer 4-phenyl-6— Chlorine 1, 2, 3, 4-an inseparable mixture of tetrahydro one ketone with a yield of 53%, convert it to oxime and separate it. (Read the precautions on the back before filling this page) Printed by the Employees ’Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs B. 4 one (3-atmosphere phenyl) one 1. 2. 3. 4 · — four gas stupid 1 _ _ oxime M. P. 129 — 1311C, 28% yield . JH-NMR (δ, CDC13): 1. 56 (bs, this paper is again used in the BB home sample standard (CNS> A 4 specifications (210 X 297 ) -79 91, 'λΚ .. A6 B6 Printed by the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention description (1 Η) f 2 • 0 — 2 • 3 (mf 2 H) »2 • 7 — 2 • 9 (m »2 H)» 4 • 1 8 (m $ 1 H) 6 * 8-7 • 4 and 8 • 0 (m 9 8 Η) Ο 13 C-NMR (δ »CD c 1 3) • • 2 1 2, 2 9 • 3 »4 4 • 8 9 1 2 4 • 2 9 1 2 6 • 7 t 1 2 7 • 2 t 1 2 8 • 6 9 1 2 9 • 3 9 1 2 9 • 8» 1 3 0 • 7 t 1 3 4 ♦ 5 9 1 4 0 • 7 t 1 4 6 • 0 t 1 5 4 • 9 0 IR (C m -1 »κ Β Γ) • • 1 5 9 8 (c — N ) o MS (%): 2 7 1/2 7 3 (Parent »C 1 3 5 / C 1 3 7 t 1 0 0/3 5) t 2 5 4 (4 2) 9 2 1 7 (2 4 ) 9 1 9 0 (2 9) ο Analysis and calculation c 1 6 Η 2 4 Ν 0 C 1 • • C 7 0 • 7 2 f H 5 • 1 9 »N 5 • 1 5 ο Experiment • C 7 0 • 7 0 f H 5 • 0 1 N 5 • 2 2 0 c • 4 benzene 6 cyanide 1 «2 • 3« 4 tetrahydro certain 1 — ketone Oil 27% yield Ο--NMR (δ, CDC: l 3) 2 • 0 — 2 • 3 (m »2 H) 9 2 • 7 7 (t 9 J = 7 9 2 H) 9 4 • 0 7 (m 9 1 H) 9 6 8 a 7 • 3 and 7 * 8 6 (m 8 H) (3-gas phenyl) compounds: (Please read the precautions on the back before filling this page) This paper size is applicable China National Standards (CNS) Grade A 4 specifications (210 X 297 mm) -80 A6 B6 Printed by the Central Ministry of Economic Affairs Standard Resident Consumer Cooperatives Fifth, Invention Instructions (78) D. 5-(3 Benzene 1 2 • 3 • 4 • 5 one four radon one 1 Η-(1) benzodiazepine 2 _ preparation method as in Example 2 2 9 Μ • P • 1 7 4 — 1 7 6 t: 9 yield 5 1 analytical calculation C 1 6 Η 1 4 N 0 C 1 • C 7 0 • 7 2 9 Η 5 • 19, Ν 5 • 1 5 〇 experiment ♦ • C 7 0 • 9 0 t Η 4 • 9 0, Ν 5 • 0 2 〇Ε. 3-bromine 5 (3 benzophenone) 2 • 3 «4 • 5 four gas 1 Η (1) benzene leather 2 ketone M. Ρ. 1 5 4-1 5 8 t: 5 1% yield Ο Analysis and calculation C 16 Η 1 3 N 〇B Γ C 1 C 5 4 • 8 1 f Η 3. 7 4 t N 3 ♦ 9 9 〇 Experiment • C 5 5 • 4 8 (+ 0.6 7) 9 Η 3 * 4 6 &gt; Ν 3 • 8 7 Ο F. Ν-the second τ hua 2 3 carries 2 oxygen 5 (3 cyanobenzene). 2 • 3 4 «5 mmlm four 1 Η (1) Benzene 氤 杂 m_l —A certain ethyl acetate amine M .P * 1 4 8--1 5 2 ° C (leukcyclohexane) »5 7% yield 〇Analysis calculation C 2 2 W 2 4Ν 2 0 2 B r C 1 ♦] L / 2 Ring: Hexane: C 5 9. 3 6, H 5 .9 8, N 5. 5 4 Ο Experiment: C 5 9. 2 6, H 6 .1 6, N 5. 5 4 Ο (Please read the precautions on the back before filling in this page) This paper scale is applicable to China National Standards (CNS) A4 specifications (210 X 297 mm) -81 Printed by the Central Standard of the Ministry of Economic Affairs, A-6 _Β6_ Five Description of the invention (79) GN—Third Dingmou 2— 卩 3-—Gas 2—Argon 5— (3-Gasyl) -2. 3. 4. 5-Siqi 1H — (1) Rong #Argoheteroyl 1 1 Z Z Zincamide M.P. 132-135t :, 72.5% yield. Analysis and calculation of C 22H hN 3〇 2C 1: C 6 2. 0 4, Η 5. 6 8, Ν 16. 44. Experiment: C 62. 12, Η 5. 5 6, N 16.510 Η. Ν-the third butyl 2-卩 3-amine-2-oxygen-5-(3-gas Rongji)-2. 3. 4 . 5 — Siqiyi 1Η — (1) Rong # Μ 杂 壳 -11-yl] acetamide acetate with 1 equivalent of triphenylphosphine and water in tetrahydrofuran at room temperature overnight. Foam was produced in 95% yield. HRMS calculation C22H27N3〇2C 1: 400. 1786. Experiment: 400. 17876. I. N — Zuo Sanding 2 — Γ3 — (3_ (3 — Tian Shen even) gland base) one 2-gas — 5 — (3 — gas stupid base) — 2. 3. 4. 5 — four argon one 1H_ (1) Benzene Gas-Leather 11-1 A single diastereomer prepared from an amine-based sleep amine, producing a diastereomer corresponding to the lower polar isomer in Example 22K , JH — NMR (δ, CDC13, TFA): 1. 33 (s, 9 Η), 2. 33 (s, 3 Η), 2.79 (m, this paper scale is applicable to China National Standard (CNS) A 4 Specifications (210 X 297 mm) -g2 (please read the $ item on the back and then write this page) — Pack · Order ... 'fruit. A6 B6

V. Description of the invention (80) I Η) $ 2 ♦ 9 6 (mfl H) 9 3 • 3 3 (AB 9 t JAB = l 6 9 △ u = = I .50, 2 H) t 4. 2 2 ( m, I Η) 9 4 • 5 8 (mfl H) P 6 • 7 — 7 • 5 (m, I 5 Η) 〇I 3 c NMR (δ t CDC l 3 »TFA) • 2 0 * 7 &gt; 2 8 • 0 3 6 »3 t 4 3 * 4» 5 0 • 5, 5 3 * 4 t 5 3 • 5% l 2 l • 4 »l 2 4» 2 9 I 2 4 • 8 tl 2 5 «L% l 2 5 • 9 $ l 2 7 • 2 $ I 2 8 • 6 tl 2 9 • 5 fl 2 9 • 8% l 3 0 • 0 $ I 3 I • 0 tl 3 4 • ltl 3 4 • 8 tl 3 7 • 2 »I 3 9 • 2 tl 4 0 • 6» l 4 2 • 7 »l 5 8 • 2 9 I 6 9 • ltl 7 3 • 6 o IR (cm -I» KB Γ) • • l 6 4 0 width (C = 0) o FABM s (%) 5 3 3/5 3 5 (Parent 9 C l 3 5 / C l 3 7 f 3 2 / l 3) $ l 5 5 (4 6) t I l 9 (l 0 0) il 0 3 (4 5) 〇Analysis calculation c 3 0 H 2 2 N 4 0 3 C l ♦ l / 3 H 2 0:: c 66. 84, Η 6. 2 9, Ν 10. 39. Experiment: C (Please read the precautions on the back before filling in this page) Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 2 3ο 1 ± Ν 5 2 6 Η, ο 9 6 6 6 2 Examples Shi Fen

2 A certain third third IN 3 3 0 a certain atmosphere I 3 base Η 5 I gas 1 2 argon four 1 5 4 3 2 I \ J # a certain atmosphere / (\ M heteroxenonyl amine ethyl acetate TJ a certain paper size Applicable to China National Standard (CNS) Grade 4 (210 X 297 mm) -83

♦., · AO 1_B6 V. Description of the invention (81) (Please read the precautions on the back before filling in this page) It is prepared from one of the diastereomers of the amine compound, resulting in a lower polarity corresponding to Example 22K Diastereomers, M.P. 240 — Printed by the Employees ’Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 2 4 3 V &gt; 8 4% yield 〇2 Η--NMR (δ, CDC 1 3 f TFA) • 1 • 3 3 (S f 9 H) 9 2 • 7 9 (mf 1 H) t 3 • 0 2 (mf 1 Η) $ 3 • 3 4 (AB 9 * JAB = 1 6 t △ v-= 1 .43 t 2 Η) 9 4 • 2 6 (m 9 1 H) t 4 • 5 9 (mt 1 H) t 6 • 7 — 7 • 5 (m &gt; 1 6 H) o 1 3 C — NMR ( δ 9 c DC 1 3, TFA) 2 7 • 8 9 3 6 • 6 4 3 • 3 9 4 4 • 0 9 5 0 • 3 9 5 3 • 4 t 5 3 • 5 t 1 2 1 • 2 * 1 2 3 • 4 t 1 2 4 • 2 negative 1 2 4 * 7 »1 2 6 • 0 9 1 2 6 • 8 9 1 2 7 • 2 f 1 2 9 • 5 t 1 2 9 • 9 9 1 3 0 • 0 9 1 3 0 • 7 * 1 3 1 • 1 * 1 3 4 • 8 t 1 3 5 • 5 t 1 3 6 • 4 f 1 3 7 • 2 t 1 3 9 • 2 t 1 4 2 • 7 f 1 5 7 »3» 1 6 9 • 1 &gt; 1 7 3 • 9 o IR (cm -1 t KB r) ♦ ♦ 1 6 4 0 width (C = 0) o FABM s (96) • 5 5 3/5 5 4/5 5 5/5 5 6/5 5 7 (Parent + 1 &gt; C 1 3 5 / C 1 3 7 »1 4/6/1 2/3/2) t 3 0 9 (1 6) »1 5 5 (6 0) t 1 3 5 (3 0) 9 1 1 9 (1 0 0), 1 0 3 (4 2) o Analytical calculation C 2 9 H 3 0 N 4 0 3 C 1 2 A &gt; 1 ./ ^ 3 H 2 0: c 6 2 • 2 6 »H 5 • 5 2 N 1 0 • 0 1 〇 Experiment • c 6 2 • 3 2 t H 5 3 8 t N 9 • 7 7 0 This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm &gt; -84 printed by FAB MS (96): 549/551 (parent, Cl35 / Cl37, 45/17), 476 (23), 21 Catch jade A6 _B6 V. Description of the invention (82) Official Example 2 7 N — 隹 三 丁某 2 — Γ3- (3 — (3 — 甲 氲 笨 某) Urea ) —2 —Argon 5 — (Qi Rongmou) — 2. 3. 4. 5 — Tetraargon-1H_ (1) Rong and 氤 杂 Η — 1 A certain Ίethine tyramine is composed of a single non-amino compound The enantiomers are prepared, yielding corresponding examples The diastereomer of the lower polar isomer of 22K, M.P. 224-227, 80% yield. ^ -NMR (δ, C Ό C \ a, TFA): 1.32

(S f 9 H) »2 • 7 7 (mf 1 H) * 2 • 9 7 (m, 1 Η) t 3 • 3 1 (AB 9 J. AB = 1 6 f △ &quot; = = 1 .57 t 2 Η) * 3 • 8 3 (st 3 H) »4 • 2 1 (m 9 1 H) t 4 • 5 5 (mi 1 H)» 6 • 7 — 7 • 5 (m 9 1 5 Η) 〇13 C-NMR (δ t CDC 1 3, TFA) 2 7 • 9 t 3 6 • 4 9 4 3 • 4 t 5 0 • 4 t 5 3 • 4, 5 5 • 5 »1 0 9» 9 t 1 1 2 • 7 9 1 1 6 • 4 9 1 2 4 • 2 f 1 2 4 • 8 9 1 2 6 «0 9 1 2 7 • 2 t 1 2 9 ♦ 4 9 1 2 9 • 9 9 1 3 0 • 0 »1 3 0 • 7 9 1 3 1 • 1 9 1 3 4 * 8 &gt; 1 3 6 • 1 f 1 3 7 • 2 &gt; 1 3 9 • 3 t 1 4 2 • 7» 1 5 7 • 7 9 1 6 9 • 1 f 1 7 3 • 8 o IR (C m -if KB Γ) • 1 6 4 0 wide (C = 0) O This paper scale is applicable to China National Standards (CNS) A 4 specifications (210 X 297 mm) -85 ---------------- (------- installed ------, 玎 ----- 7 · 4 (Please read the precautions on the back and then write the wooden page) A6 B6 Printed by the Employees Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs Description (8 net 4 0 0 (2 2), 3 2 7 (2 5), 1 5 5 (5 0), 135 (32), 119 (100), 103 (47) 〇 Analysis calculation C 33N 4〇4C 1: C 6 5. 6 3, Η 6. 0 6, Ν 10. 20. Experiment: C 65. 73, Η 6. 0 3, N 9.89. Fen Shi Example 2 8 Ν — 箆 tributyl 2 — f3 — (3 — 3— (3-ethyljuryi) ureido) — 2 — argon — 5- (atmosphere) — 2. 3. 4. 5 one to four gas ~ 1H — (1) Juxenon Phenyl-1-yl] acetamide acetate is prepared from a single diastereomer of the amine compound, resulting in a diastereomer corresponding to the lower polar isomer of Example 22K, M.P. 223-228Ό , 77% yield. 2H-NMR (δ, CDC13, TFA): 1.21 (t, J = 7, 3H), 1.32 (s, 9H), 2.63 (q, J = 7, 2 H), 2.77 (m, 1 H), 2.98 (m, lH), 3.31 (AB,, J ab = 16, Δ, = 174, 2H), 4. 23 (m, 1H), 4. 58 (m, 1 H), 6. 7 -7. 5 (m, 1 5 H) 0 / 3C-NMR (δ, CDCla, TFA): 1 4. 9, 2 7. 9, 2 8. 5, 3 6. 4, 43. 4, 50.4, 53.3, 53.4, 121.4, 123.7, 124.2, 124.8, 1 2 6. 0, (please read the precautions on the back before filling out this page) This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm ) -86 Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs _B6_ V. Description of Invention (84) 12 7.1, 127.2, 129.4, 129.9, 130.0, 131.0, 1 3 4. 5, 1 3 4. 8, 137.2 , 139.4, 142.7, 146.8, 1 5 8. 1, 1 6 9. 0, 173.7. IR (cm ·, KBr): 1640 wide (C = 0) 〇FAB MS (96): 547/549 (parent, C135 / C137, 92/35), 474 (60), 4 0 0 (5 5) , 3 2 7 (7 2), 119 (1 0 0) 〇 analysis calculation (: 3 / day 351 ^ 4〇3〇1: C 68. 06, Η 6. 45, Ν 10. 24. Experiment: C 67. 98, Η 6.35, Ν10.05〇 Fen Shi Example 2 9 A. 5 — Rongji a 7 — gas a 2. 3. 4. 5 — Tetraargon a 1H — (1) Zhu Bengzai leather 2 -Ketones such as Example 25D, prepared from the target compound of Example 25C, M.P. 184-186, 58% yield. Analytical calculations ChHhNOCI: C 70.72, Η 5.19, Ν 5. 15. Experiment: C 7 1. 0 0, Η 4. 8 6, Ν 5.07. Β. 3- Flooded 5-Juki 7-Atmosphere 2. 3. 4. 5-Tetraargon 1 1H-(1) Moxenon Miscellaneous Leather 2 — Ketone M. P. 220-22310, 56% yield. (Please read the precautions on the back before filling this page) This paper scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 *) -87 A6 B6

2109. V. Description of the invention (85) Printed analysis and calculation of the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs C i 6 Η 1 3 Ν 0 C 1 Β Γ • C 5 4 • 8 1 »Η 3 • 7 4 &gt; N 3 • 9 9 〇 Experiment • • C 6 1 • 7 9 * Η 4 • 5 7 9 N 4 • 0 9 〇C • N Dinghua 2 Γ 3 洧 2 Oxygen 5 Phenol 7 MM · Gas 2 «3 • 4 1 four gas 1 Η (1) benzene φ radon extraction 1-Hua] acetamide amine M * P • 1 2 5-1 3 〇t: (to white cyclohexyl) &gt; 6 4% yield 〇 Analysis and calculation C 2 2 Η 2 4 Ν 2 0 2 C 1 Β Γ 1/3 cyclohexane «C 5 8 • 6 1 t Η 5 • 7 4 9 N 5 • 7 0 〇 Experiment ♦ C 5 8 • 7 2 t Η 5 • 5 0, N 5 # 5 8 〇D • N th = Ding HuaZ [3 mattress radon 2 oxygen 5 benzene leather 7 gas 2 3 4 t 5 four gas 1 Η (1) benzene diazepine Leather 1 Hua] Acetylamide M ♦ P »1 6 7 1 7 0 1C ί 3 8% Yield 0 Analytical calculation C 2 2 Η 2 4 Ν 5〇2 C 1 1/3 Η 2 0:: C 6 1 • 1 8 t Η 5 • 7 6 9 Ν 1 6 • 2 1 〇 Experiment • C 6 1 • 2 8 9 Η 5 • 5 6 Ν 1 5 • 9 1 〇Ε N 丁丁华 Γ 3 Amine hua 2 Oxygen 5 Benzene leather 7 Cyanogen 2 «3 4 5 Four gas 1 Η (1) Benzyl MM leather 1 Huameng amide (Please read the precautions on the back before writing this page)

This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -QQ Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A6 __B6_ V. Description of invention (86) Foam, 65% yield HRMS calculation C22H27N3〇2Cl: 4 0 0.1786. Experiment: 400. 17952. F. N — Third Dingmou 2 — Γ3— (3 — (3_ Jiabenmou) gland group) a 2-gas-5-phenyl-7-atmosphere-2. 3. 4. 5-four argon one 1H — (1) 荣 # xenonine-1-11] 7, a single diastereomer produced from an amine-based compound, resulting in a diastereomer corresponding to the lower polar compound of Example 2 2 K Structure, 8 2% yield. &quot; H-NMR (δ, CDC13): 1. 2 4 (s, (please read the note i on the back before filling this page) 9 Η) »2 • 2 2 (s» 3 H) »2 • 7 8 (mt 1 H) »3 • 〇3 (m» 1 H) &gt; 3 • 1 8 (AB &gt; JAB = 1 6 9 △ V = 2 7 9 $ 2 H) 4 • 1 8 (m 9 1 H), 4 • 5 7 (mf 1 H) »5 • 7 6 (bst 1 H) &gt; 6 ♦ 7 — 7 • 4 (m 1 4 H) 〇1 3 C — NMR (δ t CD c 1 3 ) 4 4: 2 1 5, 2 8 ♦ 5 $ 3 6 • 9 1 4 4 • 2 9 5 0 • 1 $ 5 1 • 7, 5 3 • 5 * 1 1 6 • 9 f 1 2 0 • 7 t 1 2 3 • 8 t 1 2 6 »2 f 1 2 6 • 7 9 1 2 8 • 5 9 1 2 8« 7 »1 2 9 • 0 $ 1 3 0 ♦ 5 t 1 3 3 • 1 $ 1 3 8 • 8 t 1 3 9 • 7 t 1 4 〇 ♦ 1 9 1 4 1 • 0 »1 5 5 • 3» 1 6 7 • 2 t 1 7 2 • 6 o IR (cm -I »KB Γ) • • 1 6 4 0 wide (C = 0) O FAB MS (%): 533/535 (parent, this paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -89 V. Invention Description (87) C 1 3 5 / C 1 3 7 9 1 0 0/3 9) t 4 6 0 (7 4) , 4 0 0 (5 6) t 3 2 7 (7 2) t 1 1 9 (6 8), 1 0 7 (7 2) t 9 1 (6 7) Ο Analytical calculation C 3 0 Η 3 3 N 4 Ο 3 C 1 ♦ 1/3 Η 2〇: C 6 6 • 8 4 »Η 6 • 2 9, Ν 1 0 • 3 9 〇 Experiment: C 6 6 • 8 7 negative Η, 6. 1 9» Ν 1 0 • 1 3. w Example 3 0 N Third T Hua 2 —- “3 (5 —— (3 atmosphere phenyl) m Hua) 2 Oxygen 5 Phenyl-7 Helium 2 3« 4 .5-Four Radon 1 Η «μ ( 1) Μ. JL 氤 杂 堇 μ ··· 1 _ Hua] Ethylamine (please read the precautions on the back before filling in this page). Packed. A single diastereomer made from an amine compound, The diastereomers corresponding to the lower polar isomer of 2K in Example 2 were produced, M.P. 234_236t :, 83% yield. 2H-NMR (δ, CDC13): 1.27 (s, 9H), 2 . 8-3. 0 (m, 2H), 3. 24 (AB,, J a B = 1 6 t Δ, = 274, 2H), 4.21 (m, lH), 4.55 (m, lH),

5.76 (bs,. 1 H), 6.8-7. 5 (m, 1 3 H), 7.92 (bs, 1H) 〇23C-NMR (δ, CDC13): 28. 7, 36.6 44. 3, 50. 3, 52. 0, 53. 1, 53.5, 117.0, 1 1 9. 1, 122.4, 125.8, 126.2, 1 2 6. 9, set. Printed by the Employees Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 gongs: »·) -90 A6 _Be_ printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Description of invention (88) 1 2 8. 5, 129.0 , 129.6, 130.7, 1 3 3. 2, 1 3 4. 3, 139.6, 140.0, 1 4 0.5, 140.9, 155.0, 167.0, 17 3.0〇IR (cm- ', KBr): 1640 Broad (C = 0) O FAB MS {%): 553/554/555 / 556/557/558 (parent, Cl35 / C l37, 75/32/54/19/10), 400 (100), 3 2 7 (8 2), 2 5 4 (8 3), 2 2 8 (7 3) 〇 Analysis and calculation of CHHwNeOaC 1 2 * l / 3H2〇: C 6 2. 2 6, H 5. 5 2, N 10.01. Experiments: C 62. 49, H, 5. 40, N 9.70. Fenshi Example 3 1 N —second butyl 2 ~ Γ 3 ~ (3 — (3-tolyl) adenyl) — 2 — gas — 5 — (4 — argylphenyl) — 2. 3. 4. 5 — Tetraargon-1H — (1) Juxenoxenol-1—one] Acetamide A. 4 — (4 — Argonjule) — 1. 2. 3. 4 — Tetraargon—1 Example 22, prepared from the known 4- (4-fluorophenyl) -1, 2, 3, 4-tetrahydro one 1-ketone (see Koptyug, V. A · and Andreeva. TP ·, Zh. Organich. Kh i m. »7, 2398—2403 (1971)) See 93% yield, (please read the precautions on the back and then fill out this page) This paper scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 public goods) -91 Printed by the Employees Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs _B6_ V. Description of the invention (89) Μ.P. 154-158t: (from ethyl acetate / hexane). ^ -NMR (5, CDCla): 2.0-2.3 (m, 2H), 2.84 (m, 2H), 4. 1 3 (m, 1 H), 6. 9-7. 3 (m, 7 H), 7. 97 (m, lH), 9.36 (bs, lH) 〇 &quot; C-NMR (δ, CDCla): 21. 3, 29.5, 44.3, 115.2, 115.5, 1 2 4. 1, 1 2 7. 1, 129.2, 129.6 , 129,8. 129.9, 130.7, 139.4, 1 4 1. 4, 1 5 5. 1, 163.2. IR (called cm, KBr): 1 6 0 2 (C = N) 〇MS (96): 255 (parent, 100), 238 (42), 183 (23) 〇HRMS calculation CwHhNOF: 255. 1 0595. Experiment: 255. 10679. B. 5- (4-argon Moji)-2. 3. 4. 5-four argon-1H-(1) Zhu You Argonza 2—Picture prepared from the target compound of Example 31A as in Example 22F, yield 48%, M.P. 209—212Ό (from 2-propanol). ^ -NMR (δ, CDC13): 2.4- 2.6 (m, 4H), 4.2 (m, 1H), 6. 75 and 7.0- 7.3 (m, 8H), 8.41 (bs, lH). I3C-NMR (δ, CDCla): 32.7, (please first Read the note i on the back and fill in this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -92 A6 B6 5. Description of the invention (9〇) 3 3 • 9 »4 4 • 3 9 1 1 5 »3 &gt; 1 1 5 • 6 &gt; 1 2 2 • 0 $ 1 2 5 • 7» 1 2 7 • 4 9 1 2 8 • 5 • 1 3 0 • 2 »1 3 0 • 4 »1 3 6 • 6 t 1 3 6 • 7 9 1 3 7 • 3 t 1 6 0 • 2 f 1 6 0 • 4 t 1 7 5 • 2 o IR (cm -1 t KB Γ) • 1 6 8 0 (C = 0) o Μ S (%): 2 5 5 (parent $ 8 3) t 2 1 3 (2 9 ) t 2 0 0 (1 0 0) f 1 9 8 (5 5) »1 8 3 (2 2) 〇Analysis calculation c 1 6 H i 4 N 0 F • • C 7 5 • 2 8 9 H 5 • 5 3 9 N 5 * 4 9 O experiment • C 7 5 • 2 0 9 H 5 5 0 9 N 5 3 5 o The rest of the synthesis is the same as in Example 1: (please read the notes on the back before writing this page) Economy Printed by the Ministry of Standards and Staff Employee Consumer Cooperative C. 3 — Bromo-5 — (4-Hydroxyphenyl) — 2. 3. 4. 5 — Tetraargon—1H— (1) Benzo Xenon Leather 2—Circle M.P. 170-1801C (from methylene chloride / hexane), 58% yield, diastereomer mixture. 2H-NMR (δ, CDCla): 2.8-3.2 (m, 2H), 4.50 (m, 1 Η), 4.6 5 (m, 1H), 6. 7-7. 4 (m, 8H), 8 . 97 and 9. 23 (single peak, 1H). i3C-NMR (δ, CDCla): 43. 8, 44. 1, 44. 3, 4 5. 1, 46. 2, 4 6. 9, 115. 4, 115. 6, 115. 7, 115. 9 , This paper scale is applicable to the Chinese unitary standard (CNS> A4 specifications (210 X 297 mm) -93 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (91) 1 2 2 • 7 » 1 2 6 • 6 f 1 2 7 • 9 $ 1 2 8 • 1, 1 2 8 • 2 * 1 2 9 »1» 1 2 9 • 6 »1 2 9 • 7» 1 2 9 • 8 $ 1 3 0 • 3 &gt; 1 3 0 • 5 t 1 3 4 • 9 t 1 3 5 • 0 9 1 3 5 • 8 f 1 3 6 • 2 »1 3 6 • 6 t 1 6 0 • 4» 1 6 3 • 7 »1 6 9 • 3 9 1 7 0 • 2 o IR (C m -1 t K Β Γ) • • 1 6 9 0 (C = 0) o M S (%) • 3 3 3/3 3 5 (Parent t B Γ 7 9 / B Γ 8 1 9 4 6/5 〇) &gt; 2 5 4 (1 0 0) 9 2 0 0 (6 0) 9 1 9 8 (7 7) »1 0 9 (6 0) 〇Η R Μ S calculation C 1 6 Η 13 N 0 FB Γ • 3 3 3 • 0 1 4 6 6 Ο experiment • 3 3 3 • 0 1 4 0 9 o D • Ν = T Hua 2 Γ 3 bromine z oxygen 5 (4 fluorobenzene) 2 • 3 «4 • 5 gas l H (1) Phenanthrene leather [A Hua] amine Μ • Ρ • 2 1 5-2 2 0 V (to white cyclohexane) f 5 9% yield Ο i Η--Ν Μ R ( δ, CDC] 1 3) ·· 1 • 3 2 (st 9 Η) 9 2 • 8 — 3 • 0 (mf 2 Η) 9 4 • 2 — 4 • 6 (m 9 3 Η) f 4 * 7 7 (m $ 1 Η) t 6 ♦ 0 4 (bsf 1 Η) 6 • 6 and 7 • 0 1 7 • 4 (mf 8 H) 〇1 3 C — Ν Μ R (δ t CDC 1 3): 28. 7, 4 3 1 &gt; 4 5 8 t 4 7 0 9 5 1 6 9 5 4 ♦ 6 t 115.4, 115.7, 123.2, 127.5, (please read the precautions on the back before filling this page) This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -94 2 m A6 B6 V. Description of invention (92) 1 2 7 • 6 * 1 2 8 • 1 9 1 3 0 • 3 f 1 3 0 • 4 9 1 3 0 • 5 $ 1 3 4 • 9 9 1 3 5 • 0 t 1 3 7 • 7 t 1 4 0 • 9 9 1 6 3 • 6 9 1 6 6 • 9 »1 6 7 • 9 o IR (C m -1 f K Β Γ) • • 1 6 6 0 (c = 0) o FAB Μ s {%) • 4 4 7/4 4 9 (Parent 9 B Γ 7 9 / B r θ 1 »2 1/2 3)» 3 7 4/3 7 6 (1 0 0/9 4) t 3 4 6/3 4 8 (4 8/4 6) 2 6 6 (9 3) t 2 3 8 (4 4) ο Analysis and calculation c 2 2 H 2 4 Ν 2 0 2 Β Γ F: C 5 9 • 0 7, Η 5 • 4 1 N 6 «2 6 ο Experiment C 5 9 • 0 5, Η 5 • 1 5 9 N 6 • 2 0 ο EN second butyl 2 Γ 3 # radons oxygen 5 one (4 argon Rongmou) 2 • 3 • 4 • 5 four radon 1 H (1) cyanide leather, _ l Hua Ί 酹 acetamide M. P. 75-85¾, a mixture of diastereomers, 92% yield. (Please read the precautions on the back before writing this page again.) • Installed • Printed by the Ministry of Economic Affairs, Central Standards Bureau, S Industry and Consumer Cooperatives ^ -NMR (δ, CDC13): 1.28, 1.32 (s's, 9H), 2.4 -2.9 (m, 2H and some 2H signals), 3. 6, 3. 77, 3. 91, 4. 12, 4. 32, and 4. 69 (multiple lines of 2H and other 2H messages), 6 . 0 (broad single peak, 1H), 6.6 and 6.8-7. 4 (m, 8 Η) 〇 &quot; C-NMR (5, CDC1J: 28.6, this paper scale applies Chinese national standards ( CNS> A4 specifications (210 X 297 mm) -95 A6〇1 pqt_El 5. Description of the invention (93) 3 5 • 9 9 3 9 • 9 9 4 1 • 1% 4 3 • 2 »5 1 • 6 9 5 3 • 6 t 5 4 • 5 Ρ 5 8 • 2 t 5 8 • 9 t 1 1 5 • 1 9 1 1 5 • 4 9 1 1 5 • 7 »1 2 3 • 2 f 1 2 5 • 9 9 1 2 7 • 3 »1 2 7 • 5 9 1 2 7 • 6 &gt; 1 2 7 • 7 9 1 2 7 • 8» 1 2 7 • 9 t 1 2 8 • 0 t 1 2 9 • 3 f 1 2 9 • 5 t 1 3 0 • 2 $ 1 3 0 • 3 * 1 3 0 • 4 t 1 3 5 • 1 »1 3 7 • 5» 1 3 8 * 0, 1 4 0 • 2 9 1 4 1 • 0 f 1 6 6 ♦ 9 &gt; 1 6 7 • 6 »1 6 9 • 8 t 1 7 0 • 2 Ο IR (C m -1 t Κ Β Γ) • ♦ 2 1 0 0 (Ν 3) 9 1 6 7 0 (c = 0) Ο Μ S (96) • 4 1 0 (parent + 1 9 5 5) t 3 8 4 (3 5) t 3 1 1 (1 9) »1 5 5 (5 0) f 1 1 9 (1 〇0) 9 1 0 3 (4 0) ο Η R Μ s Calculate C 2 2 Η 2 4 Ν 5 0 2 F 4 0 9 • 1 9 1 4 〇 experiment • 4 0 9 • 1 9 0 3 Ο F • Ν 2nd T Hua 2 Γ 3 m Hua 2 oxygen 5 _L4 fluorophenyl hua) «3 • 4 • 5 Four radon _ 1 H (1) stupid and 銤 杂 璪 一 1 one mou ·] ethyl acetamide (please read the notes on the back before writing this page) Ministry of Economic Affairs Central Standards Bureau Beigong Consumer Cooperative The printed diastereomer mixture is divided into ethyl acetate insolubles, M.P. 290-295t :, 32% yield, isomer A and isopropyl ether insolubles, mp 215-2251C, 32% Yield, Isomer B. This paper is again applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 g; *) -96 A6 nm; _ ^ _ JL1 V. Description of the invention (94) Isomer A: ^ H-NMR (5, CDC13): 1.26 (s, (please read the notes on the back before writing this page) Isomer B: 2H-NMR (5, CDCla): 1.26 (s,

9 Η) »2 • 4 8 (m 9 1 H) 9 2 • 7 (width S t 2 H) 9 3 • 0 3 (mt 1 H) t 3 • 9 0 (m 9 1 H)» 4 • 1 7 (AB 9 »JAB = 1 6 t D n = 2 0 $ 2 H), 4 • 8 7 (mt 1 H) &gt; 6 • 6 and 7 • 0 1 7 • 4 (m, 8 Η) Ο IR (cm -1 f KB r) • • 1 6 8 0 (C = 〇) O M S (%) • • 3 8 4 (parent + 1 »1 〇0) t 3 11 (4 4)« 2 5 5 (1 9) • 1 1 9 (2 0) O 9 H) »2 • 5 (m, 1 H) 9 3 ♦ 0 -3 • 4 (m, 2 H) f 2 • 6 1 (m 9 1 H) t 4 »1-4 .3 (m, 2 H)» 6 • 1 2 (width s &gt; 1 H) 6 .8 — 7. 4 (mt 8 H) t 8 • 7 8 (width s » 2 H) 〇13 C — NMR (d CDC 1 3) • * 2 2. 8, 2 8 • 8 t 4 3 • 2, 5 〇 • 3 »5 1 .8» 5 3 • 3, 1 1 5 • 1 »1 1 5. 4» 1 2 5 • 2, 1 2 8. 1 &gt; 1 2 8 • 2 t 1 2 9. 4 9 1 3 0 • 7, 1 3 6. 6 t 1 3 7 • 8 t 1 4 0. 1 t 1 5 9 • 7, 1 6 2. 9 t 1 6 7 • 5 »1 6 8. 7 〇IR (cm-i, KBr *): 1 6 8 0 (C = 0) 〇MS (%): 383 (Parent generation, 10), 340 (94 paper standards apply to China National Standards (CNS) A4 specifications (210 X 297 mm) -97 丄 A6 B6 V. Invention description (95) Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs Printed) 9 2 6 7 (6 5) &gt; 2 6 1 (7 9) * 2 5 5 (6 2) 9 2 3 9 (8 1) 9 2 2 4 (6 5) t 2 1 2 (1 0 0) f 1 8 8 (8 6) f 5 7 (8 0) 0 Analytical calculation C 2 2 Η 2 6 Ν 3 0 2 F ♦ H 2C 0 3 • C 6 2 • 0 1 t Η 6 • 3 3 $ N 9 • 4 3 o experiment • • C 6 2 • 0 0 $ Η 6 • 6 1 t N 9 • 3 7 o GN τ 荸 2 r 3 (3 (3 toluene) m) 2 oxygen 5 ( 4 gas benzene hua) 2 «3 • 4 • 5 four gas 1 Η (1) benzyl miscellaneous leather 1 Hua] m · • • leukoisomer B gt. Μ • P ♦ 3 0 2-3 0 7 V 9 6 9% yield 〇2 Η--NMR (δ, CDC 1 1 3 t Τ FA) • 1 • 3 4 (S t 9 Η) f 2 * 3 4 (sf 3 H) t 2 • 8 5 (m) 1 Η) t 3 • 0 3 (mf 1 H ) f 3 • 3 4 (AB 9 t JAB = 1 6 9 △ V = 1 4 7, 2 H) 9 4 • 2 7 (m $ 1 Η) 9 4 • 6 2 (mt 1 H) 9 6 • 8 — 7 • 6 (mt 1 5 Η) Ο 1 3 C-N MR (δ 9 c DC 1 3 9 TFA) • 2 0 • 4 &gt; 2 7 • 5 t 3 6 • 6 t 4 2 • 9 t 5 0 • 6 $ 5 3 • 4 9 5 3 • 6 f 1 1 5 • 2 »1 1 5 • 5» 1 2 1 • 5 * 1 2 4 • 7 »1 2 5 • 3 t 1 2 7 • 3 * 1 2 7 • 4 ref. 1 2 8 * 9 9 1 2 9 5 t 1 2 9 • 8 f (please read the precautions on the back before writing this page). Binding · Order_ This paper is also suitable for Chinese countries Standard (CNS) A 4 specifications (210 X 297 public 31 ·> -98 A62i printed by the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs ^ _ V. Invention description (96) 1 3 1. 0, 133.7, 1 3 6. 1, 1 3 7. 6, 1 3 9. 1, 140.8, 160.0, 169.2, 17 3. 5 〇IR (cm ·, KBr): 165 ◦ wide (C = 0). FAB MS (%): 516 (parent, 17), 3 4 0 (1 0 0), 2 6 7 (7 0), 2 3 9 (5 8), 212 (46) 〇 Analysis calculation CwHwlSUOaF · 1 / 3Η2〇: C 68. 95, Η 6. 49, Ν 10. 72. Experiment: C 68. 89, Η, 6. 31, Ν 10.59. From the isomer Α, Μ.Ρ. 310 — 315 ^, 55% yield. 'H-NMR (δ, CDCla, TFA): 1.35 (please read the notes on the back before writing this page) (S 9 9 Η) t 2 • 3 2 (S t 3 H), 2 • 9 3 ( m, 2 Η) f 4 • 4 — 4 • 7 (m 9 4 H), 6 • 8 and 7. 0 — 7 • 5 (m »1 5 H) o 1 3 C -N MR (δ t CD c 1 3, T FA) 4 * • »2 0 • 5 &gt; 2 7 • 7 t 4 0 • 9 t 4 1. 2 f 5 1 • 5, 5 3« 5 ♦ 5 3 • 8 »1 1 5 • 5 &gt; 11 5 • 8 &gt; 1 2 1 • 7 &gt; 1 2 2 • 6 i 1 2 5 • 4, 1 2 8 «1 t 1 2 8 • 9» 1 2 9 • 8 $ 1 2 9 • 9, 1 3 0 • 1 9 1 3 0 • 2 &gt; 1 3 3 • 6 t 1 3 3 • 7, 1 3 3 • 8 t 1 3 7 • 4 »1 3 8 • 3 9 1 4 0 • 8 , 1 5 8 • 3 f 1 6 0 • 6 t 1 6 3 • 9 »1 6 9 • 0, 1 7 3 • 8 o The paper size is applicable to China® Home Standard (CNS) Grade 4 (210 X 297 Cli) -99 A6 B6 2, 2_5, Invention description (97) (Please read the notes on the back before writing this page) IR (cm-2, KBr): 1650 wide (C = 0) 〇FAB MS (96): 517 (parent +1, 2), 3 0 9 (1 5), 1 8 5 (2 0), 155 (5 8), 1 3 5 ( 4 5), 119 (1 0 0), 103 (5 7) 〇 analysis calculation CwHwN ^ rOaF · H2C〇3: C 65. 81, Η 6. 3 4, Ν 10. 07. Experiment: C 65. 63, Η, 6. 07, Ν 10.36. Fen Shi Example 3 2 Ν—third butyl 2-—3- (3- (3- (aerosulfur) adenyl) —2-chloro-5— (4-monochlorobenzene) —2. 3. 4. 5 -Tetraargon-1H — (1) Benzo-gas mixture leather-1 1-Acetylacetamide prepared from Example 3 One of the 1 F isomers: from isomers B, Μ.P. 271-2731C, 78% Yield.'H-NMR (δ, CDCl ^, TFA): 1.35 (s, 9 H), 2.84 (m, 1H), 3.05 (m, 1H), 3.35 (AB, , J λb = 1 6, A v = 139 Printed by the Central Standards Bureau of the Ministry of Economic Affairs and the Consumer Cooperative) H 1, H 5 co 1 1 D.,, C 3 mE, 4 ((5, 0 6 (8 3. R. • 7 M 6 4-N 3, 8 I,) · c 5 H6Z. 2, 7 ») 2 H rH 9 m / fv 4 6 • 4

AFT 4 * 3 5 5 o 5, 3 5. • 7 12 2 1 1 · &gt; 1 5.. 7 5 2 1x 1 », 7 3. .4 5 2 1X 1 ± 1,, 7 8. .3 3 2 51 This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 g; t) -100 A6 η Λ ^ _ / 3 -1- V. Description of invention ((Please read the precautions on the back first (Fill in this page) 127. 4, 129. 5, 129. 8, 130. 7, 1 3 1. 0, 135.5, 1 3 6. 0, 137.7, 1 3 9. 1, 157.5, 160.0, 163.3, 1 6 9. 3, 1 7 3. 9 〇IR (cm-, KBr *): 1650 wide (C = 0) 〇FAB MS (%): 536 (parent, 5.5), 3 4 0 (7 6) , 2 6 7 (6 5), 2 3 9 (1 0 0), 2 1 2 (7 6), 127 (7 1) 〇 Analysis calculation C23H3 &lt; JN4〇3FC 1 1/3 Η2〇: C 64. 14 , Η 5. 6 9, Ν 10. 32. Experiment: C 64. 31, Η, 5. 70, Ν 9.92〇 from the isomers Α, Μ. Ρ. 324-328t :, 28% yield. 'H-NMR (δ, CDCla): 1. 20 (s, 9 Η printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs) t 2 .0 3 (m, 1 H), 2 • 7 5 (m, 1 H ) &gt; 4 • 1 8 (m »1 H) 9 4 .4 6 (ABQ 9 J Λ B = 1 6 f △ V = 1 4 6), 2 H), 5 • 1 6 (m, 1 H) f 6 * 5-7.7 and 9. 1 7 (m 1 5 H) OIR (cm -1, KB r): 1 6 5 0 width (c = 0) OFABM s (96) 5 3 7 (parent f 1 0) 3 0 9 (1 2) 9 2 3 3 (2 5) t 1 5 5 (7 1) t 1 3 5 (6 8) 119 (1 0 0) 9 1 0 3 (8 3) o HRMS calculated C 2 s H 3 0 N 4 0 3 F c 1: 537.2062. Experiment: 537. 2056 This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -101 A6 B6 5. Description of the invention (99) Analysis and calculation C29H3〇N4〇3FC1 · 2Η2 (: 〇3: C 56. 32, Η 5. 1 8, Ν 8. 48. Experiment: C 5 6. 87 (+0.55), Η 4. 9 8, Ν 8. 8 6 〇 Fang Shi Example 3 3 Ν — 箆Sanding 2— Γ3— (3— (3-Methylarginyl) adenyl) —2 — gas—5 — (4-gas phenyl) —2.3.4.5 5 —tetraargon—1Η- ( 1) Zhuxenoxane leather 1 1 1 1 ethyl oxalolamine One of the isomers from Example 31F: from the isomer B, M.P. 275-284¾, 60% yield. ^ -NMR (δ , C Ό C \ 3, TFA): 1. 33 (Please read the precautions on the back before filling in this page) Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (S f 9 Η) »2 • 8 2 (m I 1 H) f 3 • 0 1 (mt 1 Η) »3 • 3 4 (ABQ $ JAB = 1 6 t △ If = 1 5 〇» 2 Η) t 3 • 8 7 (s 9 3 H) 9 4 • 2 6 (mf 1 H) 4 • 6 1 (m 9 1 H) f 6 • 8-7 • 5 (m * 1 5 H) Ο 1 3 C — NMR (δ 9 c DC 1 3 t T FA) 2 7 • 6 $ 3 6 • 6 t 4 3 • 0 9 5 0 • 5, 5 3 • 3 &gt; 5 3 • 7 t 5 5 ♦ 6 * 1 1 5 • 2 9 1 1 5 • 5 f 1 2 4 • 7 9 1 2 7 • 3 9 1 2 7 • 4 9 1 2 9 • 4 9 1 2 9 • 8 t 1 3 0 • 7 t 1 3 1 • 0 &gt; 1 3 6 • 1 t 1 3 7 • 7 »1 3 9 • 1 t 1 5 7 • 8 9 1 6 0 • 0 t 1 6 3 • 2 f 1 6 9 2 f 1 7 3 7 O This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -102 A6 B6 5. Description of the invention (10¾ IR (cm ·, KBr): 1650 wide (C = 0). MS (96): 532 (parent, 10), 340 (1 0 0), 2 6 7 (9 1), 2 3 9 (9 2), 212 (8 4). Analysis and calculation of C3 (&gt; H33N4〇4F · l / 3H2〇: C 6 6. 9 0, Η 6. 3 0, Ν 10. 40. Experiment: C 67.09, Η, 6. 08, Ν 10.27. From Isomer A, Μ.Ρ. 317-320TC, 21% yield. ^-NMR (δ, CD3SOCD3): 1.20 (s, 9H), 2.16 (m, lH), 2.91 (m, 1H), 3 .66 (s, 3 Η), 4. 22 (m, 1 Η), 4.47 (ΑΒ,, J αβ = 16, Δ, = 146, 2Η), 5. 10 (m, 1 Η), 6.4-6.8, 7.0-7.5, 7.73, and 8.91 (m, 15Η). IR (cm-, KBr): 1650 wide (C = 0) 0 MS (96) : 532 (parents, 5), 340 (68), 2 6 7 (7 7), 2 3 9 (8 6), 212 (6 6), 1 8 8 (4 4), 149 (1 0 0) , 123 (7 2) 〇 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the precautions on the back before filling in this page) HRMS calculation C3〇H34N4〇4F: 533. 2556. Experiment: 533. 2518.

Analysis and calculation · 2H2C〇3: C 5 7. 1 4, H 5. 5 4, N 8. 33. Experiment: C 57. 47, H, 5. 25, N 8.89 (This paper scale is applicable to Chinese National Standard (CNS> A4 specifications (210 X 297 mm) -103 A6 21? Μ: ι-^-V. Invention Description (1〇i (please read the precautions on the back and then fill out this page) + Ο. 5 6) 〇 Endeavor Example 3 4 Ν — 箆 三 丁某 2 — Γ3_ (3-(3 — 甲 笨 基) _ A) a 2 —hydrogen 5 — (2 — fluorobenz) a 2. 3. 4. 5 — four argon a 1Η- (1) 荣 #Argan 箪 一 1 a certain 1 acetamide A. 4 — (2-Argonyl) -1 1. 2. 3. 4—Siqi Li-1-ketooxime, for example, 31 is prepared from the known 4- (2-gas phenyl) -1, 2, 3, 4-—tetrahydro Guo-1-ketone (see Koptyug, VA and An dreeva, TP. Zh. Organich. Khim., 7, 2 3 9 8 —. 2403 (1971)) 90% yield, M. P. 118 — 1 2 2 t: (from ethyl acetate / hexane). Analytical calculation of Ci6Hi4N0F: C 75.28, Η 5.53, Ν 5.49. Experiment: C 74.84, Η 5.25, N 5.71. B. 5 — (2-Hydroxyphenyl) -2, 3. 4. 5 — Four gas one 1H-(1) Benzene gas leather 2-Simplified by the Ministry of Economic Affairs Central Standards Bureau employee consumer cooperative printing as in Example 31 Since Example 34 A's compound, 43% yield, M.P. 210-213t: (from 2-propanol). Analysis and calculation of CuHhNOF: C 75.28, Η5.5.3, Ν5.49. Experiment: C 75. 30, Η 5. 5 3, Ν 5.41. -104 This paper scale is applicable to the national standard (CNS) A 4 specifications (210 X 297 mm) of the country t A6 B6 V. Invention description (l〇i The rest of the synthesis is the same as example 1 :

C. 3-? Austria—5- (2-pro-cage base) —2. 3 4. 5. —Siqiyi 1Η ~ · (1) Benyouqiza 31— 2 ~~ K Μ. Ρ. 208 — 214¾ (from Erge Methane / hexane), 48% yield, mixture of diastereomers. Analysis and calculation of C / eHnNOFBr: C 57. 51, Η (please read the 1 * ^ face note first and then write this page) -install D. Ν-third butyl 2 "3-Tongyi 2-Nitrogen-5 -(2 monohydrophenyl) -2. 3. 4. 5-tetrahydro-1H-(1) i-pyrazine-1 monoyl] acetamide acetic acid M. P. 8 5-9 0 t: ( (From isopropyl ether / hexane), 100% yield. HRMS calculation ΟηΗηΒγ FN2〇2: 446. 0999. Experiment: 446. 10136. Order 3.9. 2 2, N 4. 1 9. Experiment: C 5 7. 6 0, Η 3. 6 6, N 4. 3 5 〇 Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs E. N-first-butyl 2 [3-ft gas 2-gas_5- (2-Argonyl)-2. 3, 4, 5-tetrahedron-1H-(1) Rongyou Xenon Cyanine-1-1 Acetoamide diastereomer mixture, 80% yield. HRMS calculation C22HwN5〇2F: 409. 1 9 14 .Experiment: 409. 19362. This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -105 Printed by the Employees Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A6 ^-V. Description of the invention (10¾ F. N-tert-butyl 2 [3-amino-2-gas-1 5- (2-argon Rongmou)-2. 3.4. 5 Tetraargon-1H— (1) Benzene # xenon heteroyl-1-1-acetamide Acetylacetate from a mixture of diastereomers, crystallized from the ethyl acetate monoisomeric isomer, M.P. 190—195t :, 22% yield. Analytical calculation of C22H2eN3〇2F: C 6 8. 91, Η 6.8 3, Ν 10. 96. Experiment: C 68. 93, Η 6.8 1, Ν 10.90. G. Ν — Zuo Sanding 2— Γ3— (3 — (3-tolyl) ureido) —2-argon—5- (2-—arginyl) —2, 3,4, 5 —tetraargon-1H— (1 ) Zeropyrrolidine-1-yl] acetamide acetate obtains an isomer from the target compound of Example 34F, M.P. 285-300t :, 79% yield. 2H-NMR (δ, C Ό CI 3 , TFA): 1.35 (s, 9H), 2.34 (s, 3H), 2.71 (m, 1 H), 3.0 2 (m, 1H), 3. 44 (AB ,, J ab = 1 7 , A u = 230, 2H), 4. 48 (m, 1 H), 4. 62 (m, 1 H), 6. 8-7. 6 (m, 1 5 H) 23C-NMR (d, CDCla): 20. 5, 27. 6, 37. 0, 39. 5, 50. 8, 53. 6, 5 3.7, 116. 1, 116.4, 121.4, (please read the notes on the back before writing Page). Binding. Order, In. This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -106 A6 Printed by the R-Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of Invention (1〇i 1 2 3 • 7 9 1 2 4 • 0 t 1 2 5 • 1 »1 2 6 • 2 1 1 2 7 • 9 t 1 2 8 • 7 9 1 2 9 • 1 1 1 2 9 • 2 t 1 2 9 • 3 f 1 2 9 • 5 * 1 2 9 • 8 »1 3 1 • 7 t 1 3 6 • 1 t 1 3 8 • 8 f 1 4 0 • 7 f 1 6 9 • 2 9 1 7 3 • 7 to IR (C m -1 »KB Γ) • • 1 6 5 0 width (C = 0) OFABMS (%) • 5 1 7 (Parent + 1 f 5 6), 3 1 1 (5 5) t 2 5 5 (4 7) »2 1 2 (4 2) $ 1 1 9 (1 0 0) 〇Analysis calculation c 3 0 H 3 3 N 4 0 3 FC 7 〇 • 3 3 9 H 6 • 4 4 9 N 1 0 • 8 5 o Experiment «C 7 0 • 3 0, H 6 2 8» N 1 0 • 8 5 o 3 5 N-liar $ 2-[3-"3-(3 -azabenzene *) adenyl)-2-atmosphere-5- (2-gas phenyl)-2. 3. 4. 5-four argon one 1H- (]) Rong-Biao-heteroyl-1-yl] 7, hexamethylenediamine to give an isomer, M.P. 270-283t :, 82% yield. 2H-NMR (δ, C Ό C \ 3, TFA): 1. 36 (s, 9 Η), 2. 72 (m, 1 Η), 3. 04 (m, 1H), 3. 55 (AB, , J ab = 1 7, A v = 219, 2 H), 4. 50 (m, 1 H), 4. 64 (m, 1 H), 6.8-7.6 (m, 15H). (Please read the back first Please pay attention to this page and write this page) -Installation _ This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -107 A6 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 1 3 C-NMR (dtc DC 1 3 9 TFA) «« 2 7 • 6 3 7 • 2 &gt; 3 9 • 6 t 5 0 • 7 f 5 3 • 6 t 5 3 • 8 * 1 1 6 • 2 f 1 1 6 • 5 t 1 2 1 • 2 f 1 2 3 • 4 t 1 2 3 • 8 &gt; 1 2 4 • 0 t 1 2 6 • 3 9 1 2 6 • 3 f 1 2 6 • 8 f 1 2 8 • 0 9 1 2 9 • 1 f 1 2 9 • 2 t 1 2 9 • 3 9 1 2 9 • 5 t 1 3 0 • 6 9 1 3 1 • 7 t 1 3 5 • 5 &gt; 1 3 6 • 2 &gt; 1 3 8 • 9 9 1 5 7 • 4 t 1 6 9 • 3 &gt; 1 7 4 • 1 o IR (cm -1 ♦ KB r) 1 6 5 0 width (C = 0) ο FABM s (%): 5 3 7 (Parent + 1 &gt; 1 4) 9 3 1 1 (1 7) f 2 3 8 (1 6) t 1 9 5 (1 7) »1 5 5 (5 5) t 1 1 0 (1 0 0) o Analytical calculation C 2 9 H 3 0 N 4 0 3 FC 1 • • C 6 4 • 8 6 f Η 5 • 6 3 &gt; N 1 0 • 4 3 〇 experiment • • C 6 4 * 9 0 fee Η 5 • 3 8 N 1 〇 • 2 0 o evening application example 3 6 Ν-3 T Hua 2 1 Γ 3 —— (3 (3 —— methoxybenzamide) urea group) 2 oxygen 5 (2 gas benzene flower) 2 • 3 • 4 • 5 four gas 1 H (1) benzocyanide leather l Huayi drunk Acyl m is obtained from the compound of Sassafras of Example 34F as an isomer, mp 265-280Ό, 83% yield. ^ -NMR (δ, CDCla, TFA): 1.35 (s, 9 Η), 2. 74 (m, 1 Η), 3. 02 (m, (please read the notes on the back before writing this page) Paper standards are applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 mm) -108 2131) 01 A6 B6 Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention description (10fe 1 Η) »3 • 6 1 (ABQ f J Λ s = 1 6, Δ „= 229 t 2 Η)» 3 • 8 7 (s 9 3 Η) »4 • 5 2 (m» 1 H) »4 • 6 2 (m * 1 H ) f 6 • 8-7 • 5 (mt 1 5 Η) Ο 13 C-Ν Μ R (δ tc DC 1 3): 27.6, 3 7 • 0 t 3 9 • 5 t 5 0 • 7 »5 3 • 5 I 5 3 • 8 9 5 5 • 6 t 1 1 6 «4, 1 2 2 • 7 9 1 2 3 • 7 t 1 2 4 • 0 9 1 2 6 • 2 9 1 2 7 • 9 * 1 2 9 • 1 9 1 2 9 • 2 t 1 2 9 • 3 t 1 2 9 • 5 Fee 1 3 0 ♦ 7 »1 3 1 • 7 9 1 3 8 • 8 t 1 5 7 • 7 * 1 6 9 • 3 »1 7 4 • 0 Ο IR (C m • 1» KB Γ) • 1 6 5 0 width (C = 0) 〇Μ S (%) • 5 3 3 (parent + 1 f 1 5 ) t 3 1 1 (1 8) t 1 9 5 (6 0) & 1 5 5 (5 9) »1 3 5 (6 4) f 1 1 0 (1 0 0) f 1 0 3 (8 5 ) 0 Analysis calculation c 3 0 H 3 3 N 4 0 4 F ♦ 1/4 Η 2 0: C 6 7 • 0 9% H 6 • 2 9) Ν 1 0 • 4 3 Ο experiment • • c 6 7 • 1 2 t H 6 • 0 2 1 Ν 1 0 »4 2 Ο Example 3 7 Ν 丁丁华 2 3 ο» (3 (3 tolyl) m Hua) 2 Oxygen 5 (2 Hua) 2 • 3 • 4 * _ 5 Four Μ 1 Η mmmm (1) Benzene Radon Leather _ 1 _ 华 Λ mmm A. 4 one (4-gas phenyl) one 1, 2, 3. 4 * one four gas (please read first (Notes on the back and then fill out this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -109 A6 B6 Printed by the Staff Consumer Cooperative of the Central Bureau of Standards

V. Description of the invention (lot xi-1 ketone oxime as example 31 is made from the known 4 one (4 helium phenyl) one 1,2, 3,4 one tetrahydro one one one ketone (see Kopt yue ♦ V. A. and Andreeva. TP, Zh. Organich. Khi .. * 7 »2398-2403 (1971)) 79% yield, M.P. 15 0-1 5 4 it (from ethyl acetate / hexane). Analyze and calculate ChHhNOCI: C 70. 72, Η 5. 1 9, N 5. 15. Experiment: C 70. 70, Η 5. 3 7, N 5.08. B. 5-(4-a gas Zhumou)-2.4 , 5 — Tetraargon-1H- (1) Rong # Xenon-leather-2-ketone as Example 31 was prepared from the target compound of Example 37A, 31% yield, M.P. 209-2121C (from ethyl acetate / hexane Alkane). Analysis and calculation of CuHhNOCI: C70. 72, Η 5.19, N 5.15. Experiment: C 71.01, Η 5. 1 0, N 5 · 2 2 〇 The rest of the synthesis is the same as Example 1: C · 3-Ao-5 -"4-gas phenyl)-2. 3. 4, 5, one four M-1H-M) Rong Pei cocoon 2-_M. P. 194-198 it (from methane / hexane), 20% yield, diastereoisomeric compound. Analysis and calculation of ChHuNOC 1 Br · H2〇: C (Please read the notes on the back before writing this page) ί This paper size is applicable National Standard (CNS) Grade A 4 (210 X 297 mm) ~ 110 A6-V. Description of invention (10¾ Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 5 2 • 1 3, Η 4 • 1 0 9 N 3 • 8 0 〇Experiment ♦ • C 5 2 • 2 4, Η 4 • 1 0 (+ 0 • 6 6)% Ν 3 • 8 1 0 D Ν-2nd Dinghua pf Γ 3 carrying oxygen Γ 4 atmosphere benzene Base J «3% 4 * 5 Tetra radon 1 Η (1) Benzene ψ Radon leather -1 Hua 1 Acetamide M • Ρ. 1 2 0-1 3 0 t: (Come to Baihuanji) 9 7 5 % Yield 〇Analysis calculation C 2 2 Η 2 4 Ν 2 0 2 B Γ C 1 ♦ 2/3 Η 2〇 C 5 5 .5 4 9 Η 5 • 3 7 t Ν 5 • 8 9 〇 Experiment • C 5 5 .4 5 »Η 4 • 8 2 (-0 • 5 5) t N 5 • 9 3 0 Ε Ν 一 第 Τ 華 2 Γ 3 Lip radon S oxygen 5 (4 gas Zhu) 2« 3 4 9 5 Four gas 1 Η (1) Benzene ψ Wi Hybrid extraction 1 Hua 1 Acetamide Μ • Ρ. 1 5 8 — 1 6 8 t: »Diastereomer The mixture of substances 9 75% yield. Analysis and calculation of C 2 2 Η 2 4 Ν 5 0 2 c 1 ♦ 1/3 Η 2 0:: C 6 1 • 1 8, Η 5 • 7 6 9 Ν 1 6 » 2 1 0 experiment • • C 6 1 • 0 3, Η 5 ♦ 5 9 t Ν 1 5 • 8 1 〇F • Ν-the third industrial water chestnut 2 [3 m Hua 2 oxygen 5 (please read f Please fill out this page again.). Binding · The paper size is in accordance with Chinese National Standard (CNS> A4 specifications (210 X 297 mm) -111 9, V, A6 B6 V. Invention description (Chuan Bei (4 Yirong A) a 2. 3. 4. 5-tetrakis a 1H — (1) Ju # 氤 杂 基 一 1 a certain ethyl acetate insoluble in which a diastereomeric mixture is divided by a Ίethene acetamide, 13 % Yield, isomer A and isomer B: HRMS calculated C22H2 &lt; 5N3〇2C 1: 339. 1708. Experiment: 399. 16959. G. N—Third butyl 2— “3 -— (3- (3-methyljury) adenyl) —2-qi—5-(4 —atmosphere) —2. 3. 4. 5 — four Argon-1H- (1) Jupyrazine-1-1-ylacetoacetamide gives an isomer from the above isomer B, M.P. 303-3 IOC, 88% yield. ^ -NMR (δ, CDC13): 1. 33 (s, 9 Η), 2. 33 (s, 3 Η), 2. 89 (m, 1 Η), 3. 00 (m, 1H), 3. 35 (AB ,, J AB = 16, Δ, = 159, 2H), 4. 23 (m, 1H), 4.5 9 (m Η) 6.8-7.6 (m 1 Fi Η) l note 3 pages

I Stapled daisy Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy 5 I) &gt; I .183 1 3... 5 5 9 9 7 8. ♦ 2 2 3 5 0 L0tH rH 1X 1X 2 • 9 9 9 9: 0 2417 \ ly 5 3 ^ *-· · · · 1, 5 9 3 0 c 1 2 2 3 4 CD · 1X 1X 1X c 3,,,, 4 7 0 0 2δ ... (6 4 9 1 9 R · 2 2 3 3 M61X 1X ixN3 ,,,, 1, 4 7 9 0 c 7... 2 · 1 8 059 7 2 2 2 3 C \ J rH 1 1X 1 paper The scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 mm) -112 Printed by the Central Standards Bureau of the Ministry of Economic Affairs, S Industry and Consumer Cooperatives Λ Α6 ^ _ V. Invention description (lib 16 9. Ο, 173.5 〇 IR (cm ·, KBr): 1650 wide (C = 0). FAB MS (%): 356 (56), 261 (67), 188 (7 0), 133 (1 0 0), 57 (7 7) , 2 8 (9 6) 〇 Analysis and calculation of C3〇H33N4〇3C 1: C 67.60, H 6. 2 4, N 10.51. Experiment: C 67.68, H 6. 1 9, N 10.41. Example 3 8 N —Third Ding 2 — “3— (3 —Radon Rong) Urea) —2 — Argon FS- (4— Gasoline) —2. 3. 4. 5 — Four Argon 1H— (1 ) Moxenon Xanthene-1-1 1 acetamide is prepared from the isomer B of Example 37F Isomer, M.P. 304 — 30710, 36% yield. ^ -NMR (δ, CDC13, TFA): 1.32 (s, 9 Η), 2.87 (m, 1 Η), 3. 02 (m, 1H), 3. 41 (AB ,, J ^ a = 16, Δ, = 151, 2 H), 4. 23 (m, 1 H), 4. 58 (m, 1 H), 6.8 -7.6 (m, 15H). &Quot; C-NMR (δ, CDC13, TFA): 2 7. 8, 43. 1, 5 0.4, 53. 5, 1 2 4. 7, 1 2 7. 2, 1 2 8. 7, 1 2 9. 0, 1 2 9. 4, 129. 9, 130. 7, this scan to see the remaining sulfur. (Please read the precautions on page f before writing this page) This paper scale is applicable to the Chinese National Standard (CNS> A 4 specifications (210 X 297;?!>

5. Description of the invention (11I IR (cm -1 9 KB r) • • 1 6 5 0 wide (C = 0) 〇FAB Μ s (96) • 3 5 6 (4 8), 2 6 1 (4 3) t 1 8 8 (4 4) »1 5 3 (1 0 0)» 1 2 5 (4 5) »9 0 (5 2), 5 7 (6 3) t 2 8 (4 7) 〇Analysis calculation C 2 9 Η 3 0 Ν 4 0 3 C 1 2 * &gt; 1/2 Η 2 0 • • C 6 1 • 9 2 &gt; Η 5 .5 5 »Ν 9 9 6 〇 Experiment • • C 6 1 • 9 5 t Η 5 .3 1 f Ν 9 • 9 0 ο Jing Example 3 9 Ν-tert-butyl s-Γ 3 (3 (3-Methoxymethine) glamour) 2 Oxygen 5-(4 Benzene Hua) 2, 3 * 4 .5 _ four Μ 1 Η (1) benzene φ 氤 杂 皮 1 Hua 1 acetamide (please read the precautions on the back side first and then write this page) — Pack · Order _ Ministry of Economic Affairs The Central Bureau of Standards' Employees Consumer Cooperative printed an isomer prepared from the isomer B of Example 37F, M.P. 3 0 3 ― 3 0 7 t:, 65% yield o 2 Η--Ν MR ( δ, CDC 1 3 t TFA) • 1.3 2 (S »9 Η) t 2 .8 5 (mt 1 H) 3 • 〇0 (m, 1 Η) 9 3 • 3 5 (ABQ $ J Λ s = 1 6, Δ „= 1 6 1, 2 Η) 9 3 • 8 5 (s * 3 H), 4 • 2 0 (m, 1 H) 9 4 • 5 5 (m, 1 H) 9 6 • 8 -7 • 5 (m 1 1 5 Η) Ο 13 c-N MR (δ t CDC 1 3) • 2 7. 7, 3 6 • 6 f 4 1 • 3, 4 3 • 1 f 5 0 • 5 1 5 3 .4, 5 5 • 6 f 1 2 2 .7 f 1 2 4 • 7 $ 1 2 7 • 1 1 2 8 • 7 f 1 2 9. 0 $ 1 2 9 • 4 1 2 9 • 9, This paper scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 mm) 〆A6 2 air stain, · & B6 5. Invention description (11¾ 1 3 0 • 7 9 1 3 1 • 0, 1 3 3 • 1 1 3 7 • 4, 1 3 9 • 0 t 1 3 9 • 2, 1 6 9 • 1 t 1 7 3 «9, 1 7 4 • 1 Ο IR (C m -1» Κ Β r) • • 1 6 5 0 wide (C = 0) 〇 S S (%) »5 4 8 (Parent 1 1 9 2) 9 3 5 6 (3 2) t 2 8 3 (3 7), 2 5 5 (3 4) f 2 8 (1 0 0) 〇Analysis and calculation C 3 0 Η 3 3 Ν 4 0 4 C 1 ♦ 1/3 Η 2〇: C 6 4 • 9 2 »Η 6« 1 4, Ν 1 0 • 0 4 Ο Experiment: C 6 5 • 1 9 f Η 5 • 9 3, Ν 9 • 9 9 Ο Κ Example 4 0 Ν 丁丁华 ζ Γ 3 (3 (3 toluene 荸) Xi Hua) 2 oxygen 5 (4-toluene) 2 • 3 • 4, 5 Four Gases 1 Η (1) Benzene ψ ΜΜ Hide 1 Μ 菅 醴 醅 amine (please read the precautions on the back before writing this page), install, order., Quan. Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A. 4 — (4 — Jia Rongmou) — 1. 2. 3. 4 — tetrahydrorazine — 1 — subsequent from known 4 (4-tolyl) 1, 2, 3, 4 — tetrahydro A _ 1 one ketone Example 40A target compound was prepared as in Example 31 (see Koptyug, VA and Andreeva, TP, Zh. Orga-nich. Khim., 7, 2398-2403 (1971)) 94% yield , M.P. 97-llt: (from ethyl acetate / hexane). Analysis and calculation Ci7HuNO: C 8 1. 2 4, Η This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -115 V. Description of the invention (11¾ 6.8 2, N 5. 5 7 .Experiment: C 8 1. 0 3, Η 6. 6 3, N 5. 5 7 〇B • 5-(4-W Rongmou) one 2. 4. _S_ Yi Siqi Ministry of Economic Affairs Central Standards Bureau R Engineering Printed by the consumer cooperative 1 Η-(1) Rongyou gas hetero-2- ketone as in Example 31, prepared from the target compound of Example 40A, 41% yield, Μ.Ρ. 178-1811C (from ethyl acetate / Hexane). Analysis and calculation C 7H: rN0: C 8 1. 2 4, Η 6.8 2, Ν 5. 57. Experiment: C 80.80 (-0.4 4), Η 6.6 3, Ν 5. 5 1 〇 Other synthesis as in Example 1: C. -3 Yi Mo-5 — (4 Yi Jiarong even) one 2. _S. 4. 5 one four gas .. two 1 Η — _ (1) benzo Qi Xianheng 1 2 -Nor | M. Ρ. 168 — 1761C, 68% yield, a mixture of diastereomers. D · With a second Ding Hua-3 Yi Pan-;? Yi Yi 5- (4-toluene benzene)-2, 3, 4, _5 ~ four Μ-1Η- (1) Zhu and gas mixed leather-1-a certain 1 ethyl amine brewing amine M. Ρ. 128-1381C (from cyclohexane ), 56% yield. Analysis and calculation of C 23Η27Ν2Ο2B r: C 62 31 Η 6.14.Ν 6. 32. Experiment: c 6 2. 4 9, Η X 297 mm) This paper scale is applicable to the Chinese national standard (CNS> A 4 specifications (210 (please read 1 ^ surface note $ item first and then write this page)) _ _ order_ -116 A6 _B6_ V. Description of invention (lli 6. 2 1, N 6.28. Ε. Ν — second D Radical 2- "3- —M- 2 -Gas 5-(4-Monolyl)-2. 3. 4. 5-Tetraargon 1 1-(1, Benzene gas mixed leather 1 1 XY 7, The debate box is M.P. 55-651C, a mixture of diastereomers, 75% yield.

Analysis and calculation 〇23 ^ 1271 ^ 3〇2 · l / 3H2〇: C (please read the entry first and then write this page) 6 2. 13, Η 6. 7 8, Ν 1 7. 02. Experiment: C 6 7. 0 9, Η 6. 6 7, Ν 1 6. 8 1. — Pack. F · Ν—third butyl 2- “3-amine a certain 2-gas-R-. (4-tolyl) -2, 3. 4. 5-tetraargon-1H-(1) benzene And 鰤 Miscellaneous leather 1 1 1 1 1 Glucosamine diastereomer mixture is divided into ethyl acetate insolubles, mp 292-295¾, 5.4% yield, isomer A and isopropyl ether insoluble, Μ · P. 150-170t :, 12% yield, Isomer B 〇 Isomer A: HRMS calculation C23H29N3〇2: 379. 2253. Experiment: 379.22664. HRMS calculation C23H2SN3〇2: 379. 2253. Experiment : 379, 22455. Order _ &gt; Line · The Ministry of Economic Affairs, Central Standards Bureau, Employee Consumer Cooperative printed this paper standard applies to China National Standards (CNS) A 4 specifications (210 X 297 mm) -117 213901 A6 B6 V. Description of invention (11¾ G. N — 玮 三 丁某 2- "3-(3-(3-Shen Rongmou) urea) a 2-atmosphere a 5-(4 a gas cage) a 2. 3. 4. 5- Four gas-one 1H- (1) Zhu-like chrysanthemum leather one-one-one] Acetamide made from each of the isomers of Example 40F: The white isomer B t M printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs • P • 2 3 0 1 2 3 8 V * 2 9% yield 〇 i Η--NMR (δ, CDC] ί 3) • • 1 • 2 7 (st 9 Η) 9 2 • 2 1 (s »3 H) * 2« 8 0 (mt 1 H) 9 3 • 0 0 (mt 1 H) f 3 • 2 1 (ABQ f J Λ B = 1 6 9 Δ V = 2 9 6 »2 H) &gt; 4 • 2 2 (m» 1 H) »4 • 5 8 (mt 1 H) »6 • 0 7 (bst 1 H) f 6 • 3 0 (bs, 1 H) 9 6 • 8 a 7 • 4 (m ， 1 2 H) 9 7 • 6 4 (bs ♦ 1 H) o 13 C-NMR (δ * CD c 1 3) • *: 2 1 L. 4, 2 8 * 5 $ 3 7 • 1 t 4 4 • 3 9 5 0 * 1 f 5 1 • 6 »5 3 • 7 9 1 1 6 «6 f 1 2 3« 2 »1 2 3 • 5 9 1 2 7 • 1 I 1 2 7« 7 f 1 2 8 * 6 »1 2 8 • 8 t 1 2 8 • 9 9 1 2 9 • 〇9 1 3 7 • 9 9 1 3 8 • 2 9 1 3 8 • 7 t 1 3 9 • 0 t 1 4 1 • 1 9 1 5 5 «4 9 1 6 7 • 9 t 1 7 3 • 0 0 IR (cm -1 9 KB Γ) • ♦ 1 6 5 0 width (C 0) o FABM s (%) • • 5 1 3 (parent + 1 »8 2)» 4 4 0 (9 2 ) t 2 3 4 (1 0 0) 9 2 0 8 (9 6) 9 119 (85) 〇 (Please read first Please pay attention to the details before writing this page). Binding, ordering, thread. This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm). 118 Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs . A6 21 ·,】 * 丄 _B6 V. Description of the invention (HRMS calculation 5 1 2. 275 14. Experiment: 512. 27474. From isomer A, M.P. 298-305Ό, 68% yield. ^ -NMR (δ, CD3SOCD3): 1.22 ((Please read the precautions on the back before filling out this page) _Pack- Order. &Quot;

S 1 9 Η) 9 2 • 0 3 (mt 1 H) f 2 • 2 1 (s 9 3 Η) »2 • 3 1 (s 3 H) t 2 * 8 2 (m» 1 H) Ref 4 • 4 5 (ABQ f J Λ s = 1 6, Δ, = 1 3 5, 2 H) $ 4 φ 2 4 (m »1 H)» 4 • 9 9 (m 9 1 H) &gt; 6 * 5 one 7 • 3 (m »1 3 H)» 7 * 6 6 (bs &gt; 1 H) 9 8 • 6 7 (bsf 1 H) o 1 3 C — NMR (δ t CD 3 S 0 CD 3): 2 1 • 2 f 2 8 • 5 9 4 1 • 2 4 9 • 6 9 5 0 • 3 »5 1 • 1» 1 1 4 • 7 »1 1 8 1 f 1 2 2 • 0 t 1 2 3 • 0 t 1 2 5 • 9 9 1 2 6 4 & 1 2 6 • 5 t 1 2 7 • 0 »1 2 7 • 6 y 1 2 8 4 1 2 8 • 5 9 1 2 9 ♦ 4 1 3 7« 6 f 1 3 7 8 9 1 3 9 • 0 f 1 4 0 • 1 1 4 0 • 5 »1 5 4 4 9 1 6 7 • 〇t 1 7 1 • 1 o IR (cm -1 t KB Γ) 1 6 5 0 width (C = 0) ○ FABM s (%): 5 1 3 (parent + 1 t 1 0) »3 8 0 (1 0 0) 9 3 0 7 (5 6) f 1 5 5 (4 6) 1 1 1 9 (9 8) o Analytical calculation C 3 1 H 3 6 N 4 0 3 ♦ 5/4 H 2 0: C 69. 57, Η 7. 2 5, Ν 10 .47. Experiment: This paper is again applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -119 21. Such as (&gt; ί · Α6 Β6 V. Invention description (C 6 9. 5 5, Η 7. Ο 5, Ν 10.42. Example 4 1 Ν— 三 丁丁 2— “3 -— (3-—3-Rongmou) 觫 基) —2 -gas-5— (4-tolyl) —2. 3. 4. 5 — Tetraargon-1H — (1) Rongyou 氤 Misha-1-1 A certain isomer produced from Example 40F: from isomer B, M. Ρ.235 — 238t !, 65% yield. IH-NMR (δ, CDC13): 1.30 (s, (please read the note Ϋ on the back before filling in this page)-installed. Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs System 9 Η) 9 2 • 2 1 (S 9 3 H) t 3 * 〇 (mt 2 H), 3 • 3 6 (ABQ t J Λ B = L 6, Δ, = * 2 3 9, 2 H) 1 4 • 3 0 (m 9 1 H) »4 • 6 4 (m» 1 H) f 6 ♦ 7 — 7 • 5 (mt 1 3 H) t 7 • 5 7 (bsf 1 H) f 8 • 0 6 (bst 1 H) o 2 3 C —- NMR (δ »CD c 1 3) •,: 2: L. 5, 2 8 • 7 1 3 6 * 8 f 4 4 • 5 9 5 0 • 5 9 5 1 • 9, 5 3 • 2 $ 1 1 6 • 9 &gt; 1 1 9 • 0 »1 2 2 • 1 * 1 2 3 • 4 f 1 2 4« 2 »1 2 6 • 1 9 1 2 7 • 1 f 1 2 7 • 1 9 1 2 7 • 2 $ 1 2 7 • 3 9 1 2 7 • 8 t 1 2 8 • 1 t 1 2 8 * 2 t 1 2 9 • 0 t 1 2 9 ♦ 5 t 1 3 0 • 9 9 1 3 7 • 9 t 1 3 8 • 3 »1 4 0 • 7 t 1 4 1 • 1, 1 4 1 • 6 t 1 5 5 • 2 t 1 6 7 • 4 9 1 7 3 • 3 o order. Japanese. This The paper scale is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -120 A6 B6 V. Description of invention (ill Printed IR (C m -2 »K Β Γ) by Employee Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs • • 1 6 5 0 wide (C = 0) OFA Β Μ S (%) • 5 3 3 (parent + 1 $ 3 5) t 4 6 0 (6 7) &gt; 2 6 2 (3 7) 9 2 3 4 (1 0 0) t 2 0 8 (8 5) t 1 0 5 (3 6) Ο Analysis calculation c 3 0 H 3 3 Ν 4 0 3 C 1 • C 6 7 • 6 0 9 H 6 • 2 4 Ν 1 0 • 5 1 Ο Experiment · C 6 7 • 5 0 t Η 6 • 5 9 N 1 〇 • 3 4 Ο Leukoisomer A, M • Ρ • 2 5 3 — 2 6 3 V t 6 8% yield Ο 1 Η--Ν Μ R (δ, CD 3 S 0 CD 3): 1 * 2: L (S t 9 Η) 9 2 • 0 3 (m 9 1 Η) &gt; 2 • 3 1 (s »3 Η) I 2 • 7 5 (m »1 Η) t 4» 2 0 (mt 1 H) »4 • 4 4 (AB 4 f J Λ Β = =) L 6, Δ, = 1.1.6, 2 H) &gt; 4 • 9 6 (m &gt; 1 Η) »6 • 5-7 • 3 (m 9 I 3 Η)» 7 * 5 9 (b S 9 1 Η) t 8 • 1 7 (bst I Η) Ο 13 C — Ν MR (δ 9 CD α S 0 CD 3) • 2 1 • 2 f 2 8 • 4 t 1 0 6 • 9 t 1 1 5 • 5 9 1 1 5 • 6 »I 2 0 • 7 t 1 2 2 • 9 f 1 2 5 • 8 »1 2 6 • 4 &gt; I 2 7 • 0 9 1 2 7 • 1 9 1 2 8 • 3 1 2 9 • 4 &gt; I 2 9 ♦ 9 9 1 3 3 • 3 »1 3 7 • 5 1 3 9 • 2 f I 4 0 • 3 f 1 4 0 • 4» No remaining master IR (cm -1 9 K Β Γ was seen in this scan ) • • 1 6 5 0 wide (C 0) 〇FAB MS (96): 533 (parent +1, 12), (please read the notes on the back before filling in this page) The wooden paper scale is applicable to Chinese national standards ( CNS &gt; A 4 specifications (210 X 297 mm) -12 1 A6 B6 ⑼C, J_ V. Description of invention (11b 3 3 5 (1 5), 2 3 4 (2 0), 169 (6 7), 1 5 5 (3 3), 1 3 5 (4 0), 1 1 9 (1 0 0), 1 0 3 (5 7) 〇HRMS calculated C 2 3 Η 3 〇Ν 4 0 3 FC 1: 532.32319. Experiment: 532. 2312. Fen Shi Example 4 2 N — Zuo Sanding 2 — Γ3- (3 — (3-methyl argon) urea) a 2-argon 5 — (4 a methyl stupyl) one 2. 3.4. 5 one Tetraargon-1H— (1) 篆 # xenon-leather-1 1-yl 1-acetamide Acetate prepared from Example 40F Isomer B, M.P. 233-236 1C, 60% yield. (Please read the precautions on the back before filling in this page)-Installed-Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 1 Η--Ν Μ R (δ, CDC 1 [3 t TFA) • 1 • 2 7 ( S 9 9 Η) &gt; 2 ♦ 2 0 (S 3 H) »2 • 8 5 (mt 1 Η) 9 3 • 1 0 (m $ 1 H) 9 3 • 2 8 (ABQ &gt; JAB = 1 6 t Δ ν = 2 9 4 &gt; 2 H) t 3 • 6 8 (s »3 Η), 4 • 2 4 (mt 1 H) 9 4 • 6 5 (mt 1 H) 9 6 • 8 — 7 • 5 (mf 1 4 H) »7 • 8 2 (bs $ 1 Η) Ο 1 3 C — Ν Μ R (δ tc DC 1 3)« 1: 2] L. 5, 2 8 • 6 9 3 7 • 3 9 4 4 • 4 »5 0 • 2 * 5 1 • 7 9 5 3 • 6 t 5 5 * 1 f 1 0 4 • 9, 1 0 8 • 8» 1 1 1 • 6, 1 2 3 * 3 9 1 2 4 • 7 9 1 2 6 »1 f 1 2 7 • 1 1 2 7 * 1 2 7 • 7 9 1 2 7 8 t This paper size is common to China National Standard (CNS) A 4 specifications (210 X 297 Mm) -122 Orders ·

I 21-9 ° 3 5. Description of the invention (12¾ A6 B6 1 2 8 • 2 t 1 2 8 • 9 t 1 2 9. 0 »1 2 9 • 4 9 1 3 0 • 8 9 1 3 7 • 9 i 1 3 8. 3 1 4 0 • 6 $ 1 4 1 • 2 9 1 5 5 • 2, 1 6 0. 2 &gt; 1 6 7 • 5 9 1 7 3 • 0 0 IR (C m -1 9 KB Γ) • 16 5 0 width (C = 0) 〇FAB Μ s (%) • • 5 2 9 (parent + 1 t 5 0) »4 5 6 (6 8) 3 0 7 (5 0), 2 6 2 (5 0) 9 2 3 4 (1 0 0) 9 2 0 8 (9 2) 〇Analysis calculation C 3 1 H 3 6 Ν 4 0 4 • C 7 0 • 4 3 f Η 6 • 8 6 t N 1 0 • 6 0 Ο Experiment • • C 7 0 • 2 3 9 Η 7 ♦ 2 2 t N 1 0 • 3 6 0 Real MM 4 3 Ν -third τ Hua 2 Γ 3 _ (3 (3 _ benzene Hua) m Hua) 2 oxygen 5 (4 toluene hua) 2 «3 t 4« 5 four gas 1 Η (1) benzodiazepine extraction 1 1) isomers prepared by acetamide white example 4 0 F isomer B 9 Μ. Ρ «2 1 0 2 1 4 1C, 5 5% yield. (Please read the notes on the back before filling this page) Central Standard of the Ministry of Economic Affairs Bureau HIGHLAND consumer cooperatives printed

J ft / IN4 1X 1i: V) / 3c Dc t δ / TV RMNIH) HH 2 9,, 7 s H (J 6, 2 Q / IV 12) 5 H. 3 2 ft 7) 2 2 s (5 0 8 2. H 3 w H, 1; m, B (s A 3 b (2 (1 · o 3 4 9 • 9 · 3) 5, H,) 2) Η, H 13 1, 9, m 2 m (11 (7 〃 6 o △ 4 • 9 · 3 6 4 »1,) H) HilflH r-Η To This paper scale applies the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -123 2139 ^ 1 Α6 Β6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention description (i2i) t 6 • 5 4 (bst 1 H) &gt; 6 • 8 1 7 • 4 (m »1 2 Η)» 7 • 7 6 (bs 9 1 H) ο 13 C-NMR (δ »c DC 1 3) 1:16. 0, 2 0 • 9 9 2 1 ♦ 5 t 2 8 • 6» 3 7 • 2 9 4 4 • 4 f 5 0 • 3 f 5 1 • 6 $ 5 3 • 6 1 1 1 7 • 0 f 1 1 9 • 4 t 1 2 2 • 3 f 1 2 3 • 3 1 1 2 4 • 6 &gt; 1 2 6 • 2 9 1 2 7 • 2 9 1 2 7 ♦ 7 9 1 2 8 • 2 »1 2 8 • 7» 1 2 9 • 0 t 1 3 0 • 8 f 1 3 7 • 9 9 1 3 8 • 3 f 1 3 9 • 2 9 1 4 1 • 2 t 1 4 1 • 8 t 1 4 5 • 2 9 1 5 5 * 4 9 1 6 7 • 6 t 1 7 3 • 0 o IR (cm -i 9 KB Γ) 1 6 5 0 width (C = 0) o FABMS (%) • • 5 2 7 (parent + 1 &gt; 4 0) &gt; 4 5 4 (4 7) 9 3 8 0 (4 5) t 3 0 7 (6 0) t 2 6 2 (5 3) f 2 3 4 (1 0 0) f 2 0 8 (6 0) o Analytical calculation C 3 2 H 3 8 N 4 0 4 • C 7 2 • 9 8 t H 7 • 2 7 t N 1 0 • 6 4 〇Experiment · C 7 2 • 9 7 9 Η 7 • 7 4 (+ 0 • 4 7) 9 N 1 0 • 3 9 0 Η RMS calculation C 3 2 H 3 8 N 4 0 3 5 2 6 • 2 8 7 7 0 experiment • • 5 2 6 • 2 8 6 9 5 〇Sin Example 4 4 Ν _ T Thua 2 r 3 (3 (3 toluene hua m) hua) 2 Oxygen 5 (3 • 4 two gas benzene hua) _ 2 3 • 4 .5 — tetraargon-1 Η — (1) Rongyou's Miscellaneous Leather 1-A Ίacetamide (please read the precautions on the back before filling in this page) This paper size is applicable to the China® Standards (CNS> A4 specifications (210 X 297 Cli) -124-A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of Inventions (122) A. 4 · — (3. 4 Diamine Zhuji)-1. 2. 3. 4-Tetrahydropyrene-1 circle made from the known 4 1 (3, 4 -di- radon phenyl) -1, 2, 3, as in Example 3 1 A 4 — Tetrahydrol-1-one (see Qual 1 ich, GJ, Williams, Μ · Τ., Friedmann, RCJ · Org · Chem., 55, 4971-4973 (1991)) 70% yield, Μ · P . 159-162t: (from dichloromethane / hexane) Ο Analytical calculation CuHiaNOC 12: C 62. 76 · Η 4. 2 8, Ν 4.57. Experiment: C 62.41, Η 4.0 4, Ν 4.44. Β. 5 — (3. 4-two gas stupid group) one 2. 3. 4. 5 ~ four argon one 1Η — (1) Xuan Xuan Zhezao 2 2_ _ as example 31B made from the target of Example 44A Compound, 89% yield, M.P. 191-194¾. Analysis and calculation of C; eH / 3NOCl2: C 6 2. 7 6, Η 4. 2 8, Ν 4. 57. Experiment: C 62. 56, Η 4. 14, Ν 4.59. The other synthesis is the same as in Example 1: C. 3 — bromine mono 5 — (· Ί. 4 diphenyl phenyl) — 2. 3. 4, 5 — tetrahydro mono 1H — (1) Rongzhuang 鰤 皮 _2 —Keton M. P. 183 — 188 * 0 (from ethyl acetate_ / hexane) This paper scale uses the Chinese National Standard (CNS) A4 specification (210 &gt; 097 公 #)-125 '----- ----------- j -------- install ------ · 玎 ----- &lt; Please read the precautions on tMc first and then fill in this page &gt; A6 B6 Printed by the R and Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of invention (123), 73% yield, diastereomeric mixture. HRMS calculation CieHuNOBrC 1 2: 382.9477. Experiment: 382.9480. D. N-tert-butyl 2 ~ [3-? Dianyi 2-Dong—5- (_3, 4 -dihydrophenyl) -1 2. 3. 4 ·. F5 — Tetrahydro-1H — (1) 茏 妆 氤 杂 堇 _1 One very Ί Z 酴 魴 飋 胺Μ · P. 85-95, 92% yield. HRMS calculation C32H23N2〇2BrC 1 2: 496.0315. Experiment: 496. 03341. E. N — the third butyl 2 "3-? Xenon-2-argon-FS- f 3. 4-two atmosphere Rongmou) a 2. 3. 4. 5-four gas a 1 H-f 1) Rong Pei argon heteroaluminium_Ί-a certain Ί π-pyridineamine M. Ρ. 79-99t :, a mixture of diastereomers, 91% yield. HRMS calculation 〇22 ^ 1231 ^ 5〇2 (: 1 2: 459. 1225. Experiment: 459. 12421. FN—the third butyl 2 2—3-amine 2—gas 5— (3.4—dichloromethane) —3.4.5—tetraargon-1H -(1) Caiyou Xenon Zashen-1 1-Xi] Hexamethylenediamine in tetrahydrofuran aqueous solution reduced with triphenylphosphine to prepare a diastereoisomeric mixture, which is divided into isopropyl _ insoluble, Μ. 190 (Please read the precautions on the back and then this page) This paper scale is applicable to the national standard (CNS) A 4 specifications (210 X 297 mm) -126 A6 B6 V. Description of the invention (124) t :, 3 1% yield, isomer A and chloroform insoluble, M.P. 140—15010, 1.5% yield, isomer B. Isomer A: Analytical calculation C 25N 3〇12 2: C 6 0.8 3, Printed by Beigong Consumer Cooperative of Central Bureau of Standards of Ministry of Economy Η 5 • 8 0 9 Ν 9 • 6 7 〇 Experiment • c 6 0 .9 1 t Η 5 • 7 1 »Ν 9 • 4 6 o G • Ν 2nd T Hua s Γ 3 (3 (3-Tolua) m Hua) 2 oxygen (3« 4 dichlorophenyl)-2 3 4 «5 Tetra-radon 1 H (l) Benzene aza-leather 1-Hua] white compound prepared by acetamide 4 4 F one of the isomers • • leukomeric isomer B $ MP • 2 9 9 — 3 0 1 V, 58% yield 〇7 Η--NMR (δ, CD 3 S 0 CD 3) •] L. 2 3 (S f 9 Η) $ 2 • 2 1 (S f 3 Η) t 2 • 9 2 (mf 1 Η) 3 # 4 (mf 1 H) f 3 t 4 2 (AB 9 »JA a = 1 6 $ △ V = 2 2 9» 2 H) &gt; 4 • 3 5 (m, 1 H ) &gt; 4 • 5 8 (mt 1 H) 9 6 • 6 a 7 • 6 (m, 1 4 H) 9 8 «7 5 (bst 1 H) o 1 3 C — Ν Μ R (δ f CDC 1 3) 4 *: 2 1 2, 2 8 ♦ 5 9 4 2 • 8 t 4 8 * 7 * 5 0 • 3 9 5 1. 9 t 6 0 • 3 9 7 2 • 3 9 1 1 4 • 8 9 1 1 8 2 t 122.0, 1 2 4. 4, 126.9, 127.2, (please read the precautions on the back before writing this page)-丨 Install · Order-This Paper standard General Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -127 Α6 Β6 V. Invention description α25) 1 2 8 .4, 1 2 8. 5, 1 2 8. 6, 1 2 9 . 1, 1 3 0 .2, 1 3 0. 8, 1 3 6. 6, 1 3 7. 8, 1 4 0 .1, 1 4 1. 7, 1 4 4. 0, 1 5 4. 0 , 1 6 6 .8, 1 7 0. 3 〇IR (cm -1, KB r) • 16 5 0 wide (C =: 0) 〇FAB MS (96): 566/568 (parent, C135C137, 4 / 2), 390 (25), 289/2 9 1 (4 2/4 0), 261 (5 0), 188 (60), 133 (100), 57 (65) 0 HRMS calculation CwHwN ^ rOaC 1 2 : 566. 1845. Experiment: 566. 1861. From the isomer A. Μ.P. 331—33410, 90% yield (please read the notes on the three sides before filling in this page) — Pack. Order. Printed by the MEE Consumer Cooperatives, Central Standards Bureau, Ministry of Economic Affairs 2 Η --NMR (δ, CD 3 s 0 c D 3) • ♦ 1.2 | 0 (S f 9 Η) 9 2 «1 0 (m 1 H) $ 2« 2 0 (s »3 Η) &gt; 2 • 8 2 (m, 2 H) t 4 • 1 2 (m, 1 H) 9 4 • 4 6 (AB q, J Λ B: = 16, Δ, = 1 5 0, 1 2 H) 9 5 • 0 4 (mf 1 H) t 6 • 5-6 • 7 and 7. 0-7 • 8 (mt 1 4 H), 8 • 6 8 (bst 1 H) 〇IR (cm -1 9 KB r) * 1 6 5 0 width (C = 0). FABM s (96) • 5 6 7 (parent »1), 3 0 9 (6) t 2 3 3 (1 7) 9 1 5 7 (1 0 〇 ), 13 5 (2 3) »1 1 9 (5 8) f 1 〇3 (2 8) 〇 Analysis calculation C 3 0 H 3 2 N 4 0 3 C 1 2: C ei 3. 4 '9,

丨 Line I This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -128 Printed by the Consumer Labor Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs

21H90I ^ L B6 V. Description of the invention (126) Η 5. 6 8, Ν 9.87. Experiments: C 6 3.82, Η 5.6 Ο, Ν 9.60. Example 4 5 Ν —third butyl 2 — “3 — (3 — (3 —gaseous urea) urea) —2 —gas—5 — (3.4-dichlorophenyl) —2, 3 4 .5 —Four Gases 1 Η— (1) Mo and Zha Za Za 1 1 XX 1 7, 醴 醅 1 §_ Isomer A, Μ. Ρ. 329-332 ΤΟ, 8 prepared from Example 44F 6% yield. 2H-NMR (δ, CD3SOCD3): 1.20 (s, 9H), 2.08 (m, 1H), 2.80 (m, 1H), 4.20 (m , 1Η), 4.47 (ΑΒ ,, J αβ = 1 6, Δ, = 147, 2Η), 5. 10 (m, 1 Η), 6.5-7.8 (m, 1 4 Η), 8.99 (bs, 1 Η) i3C-NMR (δ, CDaSOCD ^): 28. 9, 49. 9, 50. 8, 51.4, 56. 1, 60. 7, 7 2. 7, 8 5. 2, 116.4, 117.4, 121.3, 1 2 3. 7, 1 2 7. 18, 1 2 2. 22, 1 2 8. 0, 1 2 9. 6, 1 3 0. 1, 1 3 0. 7, 1 3 1. 18, 1 3 1. 22, 1 3 3. 6, 1 3 8. 5, 1 4 0. 7, 1 4 2. 1, 1 4 2. 3, 1 5 4. 6, 167.5, 17 1. 3 〇 (please read the precautions on the back before writing this page) 丨 installed-ordered. 'Quan- This paper scale is applicable to China National Standards (CNS) A 4 specifications (210 X 297 mm) -129 A6 0 1 5. Description of the invention (127) IR (cm -2, KB Γ) • 1 6 5 0 (C = 0) 〇FABMS (96) • 3 8 5 (3 5), 2 3 3 (1 8) &gt; 1 5 5 (5 6) t 1 3 5 (3 5), 1 19 (1 0 0 ) »1 0 3 (4 4) o Analytical calculation C 2 9 H 29N 4 0 3 C 1 3: C 5 9. 2 4, Η 4 • 9 7 t N 9. 5 3 〇 Experiment • C 5 9 .52 , Η 4 • 9 2 t N 9. 2 3 〇 Fen Shi Example 4 6 N _ 三 丁丁 2 — 〔3 — (3 — (3-methylphenyl)) (Please read the notes on the f side first (Write this page) I # very urea 5I gas 1 2 a certain fragrance II 4 3

S 3 Η 1ΧI argon tetra I 5 · 4 leather heteroxenon Rong yin yi • —- ^ a certain amine

7 2 31 4 2 3 Ρ ΜA 物 榑 的 异 的 F ο 4 rate 4 production cases% white 2 system 9 V

R M N -H

Dco s 3Dc ο 2 order.: Lu.

s 1X Employee consumption cooperation of the Central Bureau of Standards of the Ministry of Economic Affairs

IX 9 2 4 7 s13 4 7,, D .0s c 1i H b, 5, J (8S 1 δ * 7 o (4 &gt; »7 (8. • 7 B m 7 R. 3 2 6 A (· Moo , · (4 8 N 5 1} 371, I,, H, 4 ·) c 8 7 9) · 5 H ^.., H 4, 4 H, 1), H m3 fl Λ ix 6 6

H • Li-4 Δ 4 co 5 3, Η m 1 / fv 9 3 m 8 (.2 2 2

Η 2, 9 4 rH m / IN 7 7 9 7 • · 9 8 0 3 2 6.:, O) 31D · 1 〇 丨 5 This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 ) -130 A6 B6 V. Description of the invention (128) 1 2 3 • 6 9 1 2 3 ♦ 7, 1 2 7 • 0 »1 2 7 • 2 &gt; Please 1 2 8 • 0 see 1 2 9« 6 , 1 3 0 • 1 f 1 3 1 * 1 9 first read 1 3 1 ♦ 2 9 1 3 1 • 7, 1 3 8 • 6 9 1 4 0 ♦ 8, note on the back 1 1 4 1 • 8 9 1 4 2 ♦ 4, 1 5 4 • 7 9 1 6 0 • 4 f 1 6 7 • 5 9 1 7 1 • 4 〇item rebirth IR (C m -1 9 KB r) 1 6 5 0 width (C = 0) 〇 scold this page Μ S (96) • 5 8 3 (parent $ 1) 9 4 5 6 (2 1) 9 2 9 3 (2 5) * 2 7 9 (2 7) $ 2 3 3 (3 9) 9 1 5 7 (1 0 〇) * 1 5 6 (9 4) 9 1 5 4 (5 3) 1 1 3 5 (6 0) $ 1 1 9 (1 0 0) S 1 0 3 (9 0) 〇Analyze and calculate C3DH32N404C 12: C 61.75, Η 5.53, Ν 9.60. Experiment: C 61.81, Η 5.35, Ν 9.37. Fen Shi Example 4 7 Ν—third butyl 2— [3 -— (3-Sheng Rongshi) ureido) —2—argon_5—phenyl—8—Shenmou—3.4.5—four gas one 1Η— (1) Stupendous xenon azarim-1—1—even 1—Ethyl Acetamide Printed by R Industry and Consumer Cooperatives, Central Standards Bureau, Ministry of Economic Affairs Hydrogen hydroxide (peariBa-nn's catalyst) in ethanol under 45ps i hydrogen is known (j. Chem. Soc., C, (1 966) 523) 8-hydroxymethyl-1 phenol After 4 hours of solution, it has a considerable yield. Μ.P. 56 — ^ 131 This paper standard uses the Chinese National Standard (CNS) A4 specification (210 X 297 mm). Printed by the Central Standards Bureau of the Ministry of Economic Affairs. Made in; 19 ":. A6 __ ___B6_ V. Description of the invention (129) B. 4-Benji-1 7-Tianmou_1. 2. 3. 4- Tetrachlorobenzyl-1 ketone and 4-benzene-1 ft—Tianmou 1. 2 · 3.4—Siqi μ-1-m Use Example 3 1 Method Koptyug, V. A · and Andreeva, Τ · P., Zh. Organich. Khin., 7, 2398-2403 ( 1971) prepared from 8-methyl-one-one ketone. Chromatographed the product on silica gel, using hexane / ethyl acetate as the elution And the separation is crystallized by formazan. The single crystal of the two compounds, which grows in methanol, X-ray analysis determines the structure of the two isomers. 7-methyl isomer, M.P. 72-74 it. ^ H-NMR (δ, CDC13): 2.2-2.8 (m, 4 Η), 2. 3 6 (s &gt; 3 Η), 4.2 5 (m, 1H), 6.8-7.4 & 7.90 (m, 8H) o &quot; C-NMR (δ, CDC13): 21.0, 32.0, 36.8, 45.0, 126.7, 126. 9, 127. 2, 128. 4, 128. 6, 1 2 9. 5, 132.6, 134.6, 143.5, 143.9, 198.4. IR (cm-, KBr): 1681 (C = 0) 〇MS (96): 336 (parent, 100), 194 (70), 165 (50) o Analysis and calculation: C27H / e〇: C 86. 40, Η 6. 82. Experiment: C 86. 39, Η 6.76. This paper is applicable to China National Standard (CNS) A 4 specifications (210 X 297 public goods) -132 --- &lt; Please read Note 4 ^ on the back and then f this page)-Binding. Order-74. Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy V. Invention Instructions (130) 8-Methyl Isomers, Μ. P. 60 — 63t :. ^ -NMR (δ, CDC \ 3): 2. 2 — 2. 7 (m 9 4 Η) 9 2 • 6 8 (s 9 3 H) 9 4 • 2 8 (m, 1 Η) t 6 • 8 -7 • 3 (mt 8 H) 〇2 3 C-Ν Μ R (δ, c DC 1 3): 23.4, 3 1 • 2 t 3 8 • 1 t 4 6 * 1 $ 1 2 6 «6 &gt; 1 2 6 • 8 9 1 2 7 • 8 t 1 2 8 • 6 t 1 3 1 • 〇, 1 3 1 • 6 t 1 3 2 • 4 t 1 4 1 • 2 f 1 4 4 • 1, 1 4 7 * 3 t 2 0 0 t 0 〇IR (cm -1 9 KB Γ) • »1 6 8 0 (C = 0) 〇 Μ S (96) • • 2 3 6 (Parent t 1 〇0 ) t 2 0 8 (8 5) 9 1 6 5 (5 0) 0 analytical calculation c 17 Η 1 6 0 • • c 8 6 • 4 0 t H 6 • 8 2 0 experiment • • C 8 6 • 7 7 t H 6 • 6 6 〇5 One Benhua one 8 One one water chestnut 2 3 * 4 «5 one four oxygen -1 —M) Rong # arganzazaiyi 2—_Xixibei C. 4 —Jumou 7 — A certain 1. 2. 3. 4 — Tetra arginine — 1 — _ is prepared from 4 — phenyl — 7 — methyl — 1, 2, 3, 4 — tetrahydrogo-1-one. Μ Ρ. 143-1461C, yield 72%. Analysis and calculation C27C / 7N〇: C 8 1. 2 4, Η 6.8 2, Ν 5. 57. Experiment: C 81. 11, Η (Please read the precautions on the back before filling out this page) 丨 Installation- Order- -Quan- This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm)- 133 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 2! _:. A6 _B6_ V. Description of the invention (131) 7.2 Ο, N 5.51. D. 5—Phenyl-8—Methylpyridine-2. 3. 4. 5—Siqiyi 1H— (1) Rong # Xenonine-2—M.P. 230—2341C, yield 28.5 %. Analyze and calculate CHCi7N0: C 81. 24, Η 6.8 2, Ν 5.57. Experiment: C 81. 25, Η 6.8 9, N 5.54. The rest of the reaction is the same as in Example 1: E. 3-"odor-5-phenyl-8-methyl-2. 3. 4. 5-four argon-1H-(1) Benyou xenon leather-2- ketone M . P. 228 — 2321C, 46% yield. Analysis and calculation CuCuNOBr · l / 4H2〇: C 6 1. 0 0, Η 4. 9 7, Ν 4. 18. Experiment: C 61.07, Η 5.0 1, Ν 4.38. F. Ν— 三 丁丁 2-“3-港 一 2- —Atmosphere 5 —Zhuji-8 —Methyl-1 2. 3. 4. 5 — 四 arg 一一 1Η-(1) 茉 # 氤 杂 箪A 1_ a certain Ίethene ethylenediamine M. P. 227-230 ^, 36% yield. HRMS calculation C23C27N2〇2Br: 4 4 2. 1249. Experiment: 442.123321. (Please read the precautions on the back first (Fill in this page) This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -134 Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A6 B6 V. Description of invention (132) G. Ν 一The third Dingping Z-r 3 one # one 2 one oxygen one decay one benzyl chrysanthemum 8 jiahua »3 .4 5 four-pack 1 Η (1) benzene φ radon mixed leather 1 extraction 1 acetamide acetate M. Ρ • 1 1 2 — 1 15 9 5 6% yield of a single diastereomer Ο Analytical calculation c 2 3 C 2 7 Ν 5 0 2 • C 6 8 • 1 3 &gt; Η 6 • 7 1 t Ν 1 7 • 2 7 〇Experiment • «C 6 8 • 4 0, Η 6 • 8 2 t Ν 1 7 # 1 2 〇Η. Ν Second Dinghua 2-Γ 3 Amine Hua 2 Oxygen 5-benzene leather 8 Jiahua 2 3, 4 • 5 tetraoxygen 1 Η (1) benzene 氲 杂 Μ 1 华] acetone acetic acid prepared ua early diastereomer corresponding to Example 4 4 isomer B, Μ • Ρ. 1 7 0-1 8 0 ° C, 75% yield 〇HR Μ S calculated C 2 3 C 2 9 N 3 0 2 • • 3 7 9 * 2 2 5 3 〇 Experiment: 3 7 9 • 2 2 6 7 0 I. Ν 丁丁华 2-Γ 3 (3 (3 toluene) adenohua) 2 Oxygen 5 Phenol 8 Amethyst 2 • 3 • 4, 5 4 Radon 1 Η (1) Benzene 1 Xenon miscellaneous leather 1 Hua 1 Acetonitrile M. P • 2 3 2 1 2 3 8 »7 2% yield 0 2 Η--Ν Μ R (δ, CDC 1 3) • • 1« 2 6 (S f 9 Η) 2 2 1 (S, 3 Η) 9 2 • 3 0 (S t 3 H), 2. 6 4 (m, 1 Η), 2. 9 2 (m, 1 Η) (please read first (Notes on the back and then write this page) This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -135 21- ^ ° A6 B6 Printed by the Industrial and Consumer Cooperatives 8 of the Central Bureau of Standards of the Ministry of Economy Description of the invention (133) 9 3 • 1 2 (AB 4 $ J Λ = 1 6, △ ν = 2 8 3, 2 Η) t 4 • 1 5 (mt 1 Η) t 4 • 5 0 (m »1 Η)» 6 • 1 0 (bsf 1 H) 9 6 • 2 one 7 • 2 (m 9 1 4 H) 〇1 3 C-NMR (δ t CDC 1 3): 21. 0, 2 1 «4 &gt; 2 8« 5 9 3 6 φ 8 »4 3 • 8 9 4 9 • 9 t 5 1 • 5 »5 3 • 6 t 1 1 6 • 3 t 1 2 0 • 0 t 1 2 3 • 4 t 1 2 5 ♦ 2 9 1 2 6 * 2 9 1 2 6 • 3 t 1 2 8 • 2 9 1 2 8 • 3 »1 2 8 • 6 * 1 3 0 • 5 $ 1 3 5 • 1 t 1 3 8 • 6 9 1 3 9 • 0 9 1 4 0 • 8 t 1 4 1 • 9 t 1 5 5 • 4 t 1 6 8 • 0 9 1 7 3 • 0 〇IR (cm -1 t K Β Γ): 1 6 4 0 width (C = 0) 〇FABM s (96) • 5 1 2 (Parent t 7 7) t 4 4 0 (1 0 0) 9 3 0 7 (7 2) 9 2 0 8 (6 8) o Analytical calculation C 3 1 H 3 6 Ν 4 0 3 • C 7 2 • 6 3 9 Η 7 • 0 8 N 1 0 ♦ 9 3 Ο Experiment • • C 7 2 • 2 9 f Η 6 • 8 5 f N 1 0 • 7 8 Ο Rich Example 4 8 N Radical Γ 3 _ (3 (3 phenyl) m Hua) 2 Oxygen 5 Phenyl 8 Methyl 2 • 3 «4 t 5 Tetrahydro 1 Η (1) Benzazepine 1 yl] Acetamide made from Example 4 7 H i Μ Ρ * 1 5 5 1 6 5 t: 9 6 8% yield. (Please read the precautions on the back before filling in this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 commonweed) -136 A6 B6 V. Description of the invention (134) 2H-NMR (δ, CDCla): 1. 2 9 (s, 9 Η printed by the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs) »2 Lu 3 3 (s» 3 Η) 9 2 • 8 1 3 • 0 (mt 2 Η) 9 3 • 3 2 (AB &lt; 1 * J Λ s = 1 6, Δ, = 2 8 5 »2 Η), 4 • 2 0 (m 1 Η) • 4 • 5 6 (m 1 H) t 6 • 6 — 7 • 3 (m, 1 3 H) »7 • 5 6 (b S 9 1 Η) 9 8 * 0 0 (bs 9 1 Η) o 1 3 c NMR (δ fc DC 1 3) 2] L. L, 2 8 7 »3 6 • 8 4 4 • 0 9 5 0 • 5 9 5 1 • 9 f 5 3 • 1 &gt; 6 0 • 4 1 1 6 ♦ 9 f 1 1 8 • 9 f 1 2 2 «0 t 1 2 4 8 9 1 2 6 • 3» 1 2 6 # 4 9 1 2 6 5 9 1 2 8 3 • 1 2 8 • 4 t 1 2 9 • 5 t 1 3 0 • 7 »1 3 4 2 t 1 3 5 • 0 f 1 3 9 • 1 9 1 4 0 • 7 t 1 4 〇8 t 1 4 2 • 0 9 1 5 5 • 2 9 1 6 7 • 4 t 1 7 3 4 o IR (cm -1 KB r) 1 6 4 0 width (C 0) 0 FABM s (96) 5 3 3/5 3 5 (parent + 1 t C 1 3 5 / C 1 3 7 f 6 9/2 6) t 4 6 0 (1 0 0) 9 3 0 7 (5 2) t 2 3 4 (6 0)% 2 0 8 (7 0) o Analytical calculation C 3 0 H 3 3 N 4 0 3 C 1 • C 6 7 • 6 0 9 H 5 • 2 4 $ N 1 0 »5 1 0 Experiment C 6 7 • 2 7 9 H 6 • 0 6 * N 1 0 • 2 3 Ο Actual travel example 4 9 5 — Benhua — 9 Yijiahuayi« 3 • 4 • 5 — Tetraoxo-1 H This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 g; *) (please read the precautions on the back before filling this page) -137 A6 B6 V. Description of the invention (135) One (1) Ju-xenon complex (please read the precautions on the back before filling in this page) For example 31, prepared from 4-phenyl-8-methyl-1, 2, 3, 4-— Four qi certain 1 one heir. A. 4-Phenyl-8-Methyl-1. 2.3.4.-Four argon baskets-1. After one ketone M.P. 130-136t :, 73% yield. Analysis and calculation Ci7Ci7NO: C 81. 24, Η 6.8 2, Ν 5.57. Experiment: C 81.19, Η 6.61, N 5.51. B. 5—Phenyl-9, a methyl group 2. 3. 4. 5—Tetraargon-1 1H— (1) Juyou M Zaco-2—Keone M. Ρ.154-157Ό, 81% yield . Analyze and calculate Ci7C77NO: C 81. 24, Η 6.8 2, Ν 5.57. Experiment: C 81.09, Η 6. 5 2, Ν 5.45. The rest of the synthesis was carried out according to Example 1. Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs C · 3-Bromo-5 — stupid one 9 a class one 2. 3. 4. B one four argon one 1H — (1) Rongpei xenon hood one 2 -_ Diastereoisomeric mixture, its one M.P. 240-243T, 44% yield. Analyze and calculate Ci / CwNOBr: C 61. 83, Η -138 This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs A 2 * A6 _B6_ V. Description of the invention (136) 4. 8 8, N 4. 24. Experiment: C 61.79, Η 4.57, Ν 4 · 0 9 〇 remaining material, 26% yield, a mixture of diastereomers, and combined with the above diastereomers in the next step . D. Ν—third T certain 2— “3—Pu Yi 2—Shovel one 5—Quan one 9 one A certain one 2. 3.4. 5—Four gas one 1Η— (1) 芏 杂 箪 一 1 one certain Separation of diastereoisomers on silica gel by Ί ZOZe, using hexane / ethyl acetate as the eluent, and then crystallizing from dichloromethane / hexane: Isomer A, M.P. 199 — 202t :, 15% yield Ο Analytical calculation C23C27N2〇2Br: C 62. 31, Η 6.14, Ν 6.32. Experiment: 0 6 2. 6 0, Η 5.87, Ν 6.12. Isomers Β, Μ.Ρ. 227-230TC, 63% yield 0 Analytical calculation C23HuN2〇2Br: C 62.31, Η 6.14, Ν 6.32. Experiment: 0 62.83 (+0.52), Η 6.48, Ν 6.22. Ε _ Ν—The third butyl 2— [3—Die 氤 一 2— 气 一 5— 荣 某 9 Yi Tian Shiyi 2. 3. 4, 5- 四 气 一 1Η — (1) Zhu # 气 杂 M-1 — Some] acetamide acetate _ This paper scale is applicable to the national standard (CNS) A 4 specifications (210 X 297 mm) ~ ~ 139 (precautions on the wf side before writing this page) Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs, Γ i A6 9, _B6_ V. Description of the invention (137) Diastereomerization Compound, which was chromatographed on silica gel, using hexane / ethyl acetate as the eluent. Isomer A, oil, 18% yield. HRMS calculation C23H27N5〇2: 405, 2 1 59. Experiment: 405.21724. Isomer B, M.P. 160-164 ^, 76% yield Ο HRMS calculation C23C27N5〇2: C 68. 13, Η 6.7.1, Ν 17. 27. Experiment: C 68. 09, Η 6. 7 1, N 17.08. F. N — Zuan tri T group 2-[3- amino group-2-argon 5-Rongji 9-A certain 2. 3. 4. 5-four Argon 1H— (1) Fuyou M Misha-1—A certain 1 ethylammonium amine from Example 4 9 The individual isomers of Ε are hydrogenated individually. Isomer A, oil. HRMS calculation C23H27N50 2: 380 1. Experiment: 380. 23462. Isomer B, oil, 13% yield. HRMS calculation C23HhN5〇2: 38〇, 233 1. Experiment: 380. 23276. G. N — 玮 三 丁某 2 — "3 — (3 — (3 — Jia Rongmou) Urea) — 2 — Argon — 5 — Seal a certain 9 A methyl a 2. 3. 4. (Please read the precautions on the back before writing this page) This The paper scale is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -140 V. Description of the invention (138) Ministry of Economic Affairs Bureau of Consumer Cooperatives printed prospective employees

Saiduo-5 «— Four 1CL one 1 H — (l) Benzene radon extract one 1 one Chinese] Acrylic acid 1 Isomers prepared above white A f M • P • 2 2 1 One 2 2 3 V» 8 4 % Yield 〇2 Η--NMR (δ, CDC 1 3) • 1 • 2 1 (S t 9 Η) »2 • 2 4 (s» 3 H) * 2 • 2 8 (st 3 H) * 2 • 7 4 (ABQ * t. J Λ B = = 16, Δ, = 13 5, 2 H) &gt; 2 • 8 2 (mf 1 H) 9 2 * 9 5 (mt 1 H) t 4 • 1 4 (mf 1 H) »4 • 5 1 (mf 1 H) t 6 • 5 4 (b S t 1 H) t 6 • 8 — 7 • 3 (mt 1 3 H)» 7 • 7 8 (b S » 1 H) o 1 3 C-NMR (δ% CDC 1 3) • * L 8.8, 2 1 • 5 »2 8 • 5 t 3 5 • 8 t 4 4 • 6 9 5 0 • 0 t 5 1 • 2 t 5 3 • 5 t 5 5 • 2 9 1 1 6 * 9 f 1 2 0 • 6 9 1 2 3 • 7 t 1 2 6 • 3 f 1 2 6 • 7 t 1 2 8 • 4 t 1 2 8 • 7 f 1 2 8 • 8 9 1 3 1 • 6 9 1 3 5 • 8 t 1 3 8 • 8 t 1 3 9 • 1 t 1 3 9 • 3 $ 1 3 9 • 9 9 1 4 1 • 3 t 1 5 5 • 4 t 1 6 8 • 0 9 1 7 4 • 7 o IR (C m -i * KB Γ) ♦ • 1 6 4 0 wide (C = 0) ○ FABM s (96) • • 5 1 3 (parent + 1 t 2 7) 9 4 4 0 (1 0 0) t 2 5 1 (3 7) f 2 3 4 (6 5) 2 0 8 (5 0) O Analytical calculation C 3iH 36N 4〇3: C 7 2. 6 3, Η This paper The standard is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -141 (please read the precautions on the back before filling this page) 01 ^ 90 X Α6 w L Β6 V. Description of the invention (139) 7. 08, N 10. 93. Inspection: C 72.89, Η 7.02.Ν 10.90. Fu Shi Example 5 0 Ν — Third butyl 2 ~ Γ 3 — (3 ~ (3-methoxybenzyl adenyl)-2-gas-5-benzene a 9 9 methyl-2. 3. 4. 5 One four gas one 1H — (1) Mozhuang arginyl group 1 A certain Ίethine alcohol amine from Example 49F Isomer A, Μ. Ρ. 162— 167 υ, 8 1% yield. JH -NMR (δ, CDC13): 1.20 (s, (please read the notes on the back before writing this page) • -install.

Printed by the Central Standards Bureau of the Ministry of Economic Affairs, 8 Industrial and Consumer Cooperatives 9 Η) t 2 ♦ 2 7 (s 9 3 H) 1 2 • 7 2 (ABQ f JAB = 1 6 f △ V = 1 4 1 t 2 H) &gt; 2 • 7 2 (mf 1 Η) »2 9 2 (m» 1 H) &gt; 3 * 7 1 (s &gt; 3 H) »4 • 2 0 (mf 1 H) t 4 ♦ 4 8 (m * 1 H) 9 6 • 5-7 • 8 (mt 1 3 H) 〇1 3 C — NMR (δ * CDC 1 3) • L 8.8, 2 8 • 5 f 3 6 • 0 9 4 4 • 5 »5 0 ♦ 0, 5 1 • 2, 5 3 • 4 f 5 5 • 2 t 1 0 5 • 3 t 1 0 9 • 2 1 1 2 • 0 f 1 2 6 • 3 t 1 2 6 • 7 t 1 2 8 • 4 9 1 2 8 • 5 t 1 2 8 * 7 f 1 2 9 • 7 t 1 3 1 • 6 f 1 3 5 • 8 f 1 3 9 • 3 t 1 3 9 • 8 t 1 4 0 «3 t 1 4 1 * 2 t 1 5 5 * 2 9 1 6 0 • 3 9 1 6 8 • 1 9 1 7 4» 6 o IR (C m • 1 f KB r) • • 1 6 4 0 Width (C = 0) O The size of the revised paper is applicable to the Chinese National Standard (CNS) Grade 4 (210 X 297 mm). I. 142 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy V. Invention Instructions (140) FAB MS (96): 529 (parent +1 , 35), 4 5 6 (1 0 0), 3 0 7 (4 4), 2 3 4 (6 2), 2 0 8 (5 4) 〇Analysis and calculation 〇31 ^^ &lt; ^ 4〇4 · 3 / 4H2〇: C 68. 68, Η 6.97, Ν 10. 33. Experiment: C 6 8. 7 4, Η 6.89.Ν 10.09. Fen Shi Example 5 1 Ν— 三 丁丁 2— “3- (3- (3—argonbenzy) ureido) —2 —gas—5 —benzy—9 —methyl—2.3.4. 5 — Tetraargon-Ί Η — (1) Fenoxenoxane-1—1—1—Ethylacetamide Prepared from Example 49F Isomer A, Μ.Ρ. 260—262 t, 77% yield. M-NMR (δ, CDCla): 1.20 (s, 9 Η) $ 2 • 3 0 (s »3 H) t 2 ♦ 8 0 (AB 9» JAB = 1 6 &gt; Δ V = 9 8 f 2 H ) f 2 • 8 — 3 • 0 (mf 2 H) t 4 ♦ 2 6 (mt 1 H) t 4 • 4 8 (m 9 1 H) f 6 • 1 7 (bs 1 H) »6 • 8 — 7 • 3 (m 9 1 2 H) 9 7 • 5 6 (bst 1 H) 9 7 • 9 6 (mt 1 H) o 13 c — NMR (δ »CD c 1 3) &lt; &lt; ► 18. 9, 2 8 • 5 t 3 5 • 6 9 4 4 • 7 t 5 0 • 2 5 1 ♦ 5 * 5 4 * 4 t 1 1 7 • 1 9 1 1 9 • 2 f 1 2 2 • 4 9 1 2 6 • 4 9 1 2 6 ♦ 7 »1 2 8 4 * 1 2 8 • 5 t This paper scale is applicable to the 0 National Standard (CNS) A 4 specifications (210 X 297 mm) -143 (please read the back first (Please fill out this page again) 2139 ^ 1. A6 B6 Ministry of Economic Affairs Printed by the Central Standard 8 Industrial and Consumer Cooperatives V. Description of Invention (141) 128.8, 129. 7, 131. 7, 134. 4, 1 3 5. 6, 139.3, 1 3 9. 8, 140.6, 1 4 1. 3, 155. 1, 1 6 7. 4, 174.7. IR (cm-, KBr): 1640 wide (C = 0) 〇FAB MS (96): 533/535 (parent, C135C137, 23/8), 460 (100), 408 (6 8), 2 3 4 (8 5), 2 0 8 (7 5). Analysis and calculation of C32H3eN4〇3Cl: C 67.60, H 6. 2 4, N 10. 51. Experiment: C 67.59, Η 6. 2 5, N 10.18. Examples 5 2 N —Third butyl 2 — “3 — (3 — (3 —Eryong) ureido) — 2 — argon — 5 — stupid 9 — methyl — 2. 3. 4. 5—Tetraargon-1H— (1) Rongyou Xenon Cinchon-1 1 XY-acetamide prepared from Example 49F Isomer A, M.P. 222 — 224 t :, 8 8% yield. ^ -NMR (δ, C Ό C \ 3): 1. 17 (t, J = 7, 3 Η), 1. 20 (s, 9 Η), 2. 28 (s, 3H), 2.55 (t, J = 7,2H), 2.72 (AB ,, J ^ = 16, = 136, 2H), 2. 76 (m, 1 H), 2. 92 (m, 1 H), 4. 20 (m, 1 H), 4. 50 (m, 1 H), 6. 60 (bs, 1 H), 6.8-7. 3 (m, 14H) 〇Winter paper scale is applicable to China National Standard (CNS) A 4 specifications ( 210 X 297 mm) —144 (please read the precautions on the back before writing this page) 丨 Install · Order · I Quan '

2l: l9〇I A6 B6 5. Description of the invention (142) 1 3 C-N MR (δ $ CD c 1 3) 4 4:] L 5. 6, 1 8 • 8 &gt; 2 8 • 5 t 2 8 • 9 »3 6 • 0» 4 4 • 5 t 5 0 • 0 parameters 5 1 • 2 t 5 5 • 4 9 1 1 7 • 4, 1 1 9 • 8 9 1 2 2 • 8 t 1 2 6 • 3 9 1 2 6 ♦ 7 f 1 2 8 • 4 t 1 2 8 ♦ 5 »1 2 8 • 7 f 1 2 8 • 9 9 1 3 1 • 6 9 1 3 5 * 8 1 3 8 • 9 &gt; 1 3 9 • 3 &gt; 1 3 9 • 9 t 1 4 1 • 2 * 1 4 5 • 4 t 1 5 5 • 3 »1 6 8 • 1 f 1 7 4 • 6 o IR (cm -i 9 KB Γ) • 1 6 4 0 width (C = 0) 〇FAB Μ S (96) • 5 2 7 (parent + 1 f 3 7) 9 4 5 4 (1 0 0) f 3 0 7 (4 5 ) 9 2 3 4 (5 4) minus 2 0 8 (4 7) o Analytical calculation C 3 2 H 3 8 N 4 0 3!: C 7 2 • 9 8 see H 7 * 2 7 &gt; Ν 1 0 ♦ 6 4 o experiment • C 7 2 • 7 7 t H 7 • 2 4 1 Ν 1 0 • 2 7 o Night Example 5 3 Ν Jiahua Third T Hua 2 _ Γ 3 (3 (3-Tolua) Urea)-s oxygen 5 (Benzene) 2 «3 • 4 -S_ 5 Tetra-1H — (1) 笨 # 气 杂 箪 一 1 base] Acetamide (Please read the precautions on the back before filling this page) Central Standards of the Ministry of Economic Affairs Printed by the living staff consumer cooperative, for example 1, made from N-methyl, N-third butyl 2- [3-amino-1 2-oxo 5- (phenyl) -1, 2, 3, 4, 5--4 Hydrogen- 1H — (1) benzoazepine-1-yl] acetamide acetate, M.P. 140-150t :, 83% yield This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -145 213901 A6 _B6_ V. Description of the invention (143) ^ -NMR (δ, CDC13): 1.30 (s, 9 Η), 2 . 19 (s, 3 Η), 2. 31 (s, 3 Η), 2.88 (m, lH), 3.15 (m, lH), 3. 32 (AB ,, JaB = 16, Δ. = 297, 2H ), 4.20 (m, lH), 4.68 (m, lH),

6. 6-7.4 (m, 1 4 H), 7. 72 (b s, 1 H

) O (Please read the precautions on the back and then f this page) Printed by WK Industrial and Consumer Cooperative, Central Bureau of Standards, Ministry of Economic Affairs

23C-NMR (δ, C Ό C \ s): 21. 5, 2 8 • 1 »3 0 • 5 t 3 8 • 1 9 4 4 • 4 9 4 9 • 8 f 5 3 • 0 f 5 7 • 4 f 1 1 6 • 9 t 1 2 0 ♦ 7 f 1 2 3 • 0 f 1 2 4 • 9 9 1 2 6 • 0 f 1 2 6 • 6 t 1 2 7 • 5 9 1 2 8 • 2 t 1 2 8 • 3 9 1 2 8 • 6 t 1 2 8 • 7 9 1 3 0 • 4, 1 3 8 3 t 1 3 8 • 9 $ 1 3 9 • 5 t 1 4 1 • 4 »1 4 2 «7 f 1 5 4 • 9 t 1 6 6 • 9 t 1 7 2 • 3 0 IR (cm -1 &KB; Γ) • • 1 6 5 0 width (C = 0) 〇FABM s (%) 5 1 3 (Parent + 1 t 4 0) »4 2 6 (1 〇0), 2 9 3 (4 2) 9 2 2 0 (4 6) f 1 9 4 (5 0) o Analysis calculation C 3 1 H 3 6 N 4 0 3 • C 7 2 • 6 3 t H 7 0 8 9 N 1 0 • 9 3 o Experiment: C 7 2 • 8 3 »H 7 • 1 6 f N 1 0 8 4 O Example 5 4 The size of the paper is in accordance with the Chinese National Standard (CNS) A4 specification (210 X 297 mm) -146 A6 B6 Printed by OK Industrial and Consumer Cooperative of Central Bureau of Standards of the Ministry of Economy V. Description of Invention (144) N Yijiahua « Third Dinghua 2 Γ 3 one (3 one (3 one Zhuhua) gland hua) 2 oxygen 5 1 benzene hua) * 3 • 4 «four gas 1 Η (1) benzyl krypton leather 1 hua 1 acetamide acetate Example 1 white Ν — Methyl, N — third butyl 2 — [3 monoamino — 2 monofluoro — 5 — (phenyl) — 2 9 3 9 4 5 tetrahydro-1 1 Η one (1) benzodiazepine -1-1 group] Acetamide t Μ • P • 1 5 5-1 6 2 t: 9 9 7% yield 0 'Η · -NMR (δ, CDC: 1 3): 1 • 3 2 (s &gt; 9 Η) »2 • 5 0 (S» 3 H) »2 • 8 4 (mf 1 Η)» 3 * 0 2 (m 9 1 Η) f 3 • 4 0 (AB 9 * j Λ Β = 1 6 △ V = 2 8 8) t 2 H) f 4 • 2 6 (m »1 Η) 9 4 • 6 2 (m 9 1 Η)» 6 »8 1 7 • 6 (mf 1 4 H) t 7 • 9 6 (b S 9 1 Η) Ο 1 3 C Ν Μ R (δ »CD c 1 3): 2 8. 2, 3 0 • 7 &gt; 3 8 • 0 9 4 4 • 5 9 4 9 • 6 »5 3 ♦ 1» 5 7 • 5 $ 1 1 7 * 4 t 1 1 8 • 9 »1 2 1 • 5 9 1 2 4 • 7» 1 2 6 • 2 »1 2 6 • 6 9 1 2 7 • 5 9 1 2 8 • 2 f 1 2 8 • 8 t 1 2 9 • 3 9 1 3 0 • 5 f 1 3 3 • 8 t 1 3 8 7 * 1 4 1 • 1 »1 4 1 • 3 t 1 4 2 • 6 $ 1 5 4 • 6 9 1 6 7 • 0 $ 1 7 2 • 8 OIR (C m -I f Κ Β Γ) 1 6 5 0 width (C = 0) o FA Β Μ s (96) 9 5 3 3 (Parent + 1 »1 4) 9 4 4 6 (8 0) t 2 9 3 (5 4)» 2 3 7 (5 2) 9 220 (98), 194 ( 100). (Please read the precautions on the back before writing this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -147 A6 B6 V. Description of invention (145) Central Bureau of Standards, Ministry of Economic Affairs Printed and analyzed by the Gonggong Consumer Cooperative Society c 3 0 Η 3 3 Ν 4 0 3 C 1 • C 6 7 • 6 0 t Η 6 • 2 4 t N 1 0 • 5 1 Ο Experiment • • C 6 7 • 7 8 f Η 6 • 2 6 t N 1 0 • 4 0 0 霣 掃 例 5 5 Ν Benzene hua • third dinghua 2-Γ 3 MM, (3 (3 ——. toluene hua)) 2 oxygen (benzene hua) • • 4 four-gas 1 H (1) benzene 氲 miscellaneous leather 1 hua 1 acid sleep amine as in Example 1 White Ν — 笮 基 9 Ν — third butyl 2-C 3 monoamine group-2 one gas 5- (Phenyl) — 2 t 3 t 4 $ 5 One tetrahydromono 1 Η — (1) Benzoazepine — 1 monoyl] Chloramine acetate 9 Μ ♦ P • 2 2 6 a 2 3 0 V * 6 3 • 5% yield Ο i Η--NMR (δ, CDC: l 3) * 1 • 3 3 (S * 9 Η) 9 2 «1 8 (S% 3 Η) &gt; 2» 8 8 (mt 1 Η) f 3 • 1 0 (mf 1 Η) t 3 ♦ 1 8 (A Β Q tj ^ B-1 6 i Λ V = 2 4 3 * 2 Η) t 4 «0 1 4 • 3 (m »3 Η) t 4 • 7 5 (m 9 1 Η) f 6 • 6 a 7 • 6 (m 9 1 4 Η) &gt; 8 • 7 5 (b S &gt; 1 Η) ο 1 3 C — Ν Μ R (δ »c DC 1 3) i: 2] L. 5, 2 8« 5 9 3 7 • 9 t 4 4 • 4 t 4 7 • 7 1 4 9 • 5 t 5 3 • 2 »5 8 • 3» 1 1 6 • 8 &gt; 1 2 0 • 4 9 1 2 2 • 9 9 1 2 5 * 5 »1 2 5 • 9» 1 2 6 • 0 t 1 2 6 • 3 t 1 2 7 «0» 1 2 7 • 1, 1 2 7 • 6 9 1 2 7 • 9 f 1 2 8 • 0 9 1 2 8 • 3 9 1 2 8 • 7 f (Please read the notes on the back first Ant writes this page) i Pack · Order--i. This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -148 A6 B6 Printed by the Employees Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Inventions Description (146) 1 2 8 • 8 t 1 2 8 • 9 &gt; 1 3 0 • 2 t 1 3 8 • 2 9 1 3 9 * 2 &gt; 1 3 9 • 4 1 4 1 • 5 f 1 4 2 • 3 f 1 5 5 • 0 9 1 6 8 * 3 * 1 7 2 • 8 Ο IR (cm -2 t KB Γ) • 1 6 5 0 width (C = 0) ο FAB Μ S (%) • 5 8 9 (parent + 1 t 1 0) 9 4 2 6 (5 4) t 2 9 3 (4 1) 9 2 2 0 (4 0) 9 9 1 (1 0 0) Ο Analysis calculation C 3 7 Η 4 0 N 4 0 3 • C 7 5 • 4 8 t Η 6 • 8 5 »N 9 • 5 2 〇Experiment C 7 5 • 0 9 9 H 6 • 8 8 f N 9 • 3 0 〇night travel example 5 6 Ν Benzene «The third butyl chestnut 2 1 ί 3 (3 (3 __ Atmosphere ) Urea Hua) 2 oxygen "Benhua) 2 • 3% 4 • 5 four gas 1 H (1) benzoazepine leather 1 Hua 1 acetamide as in Example 1 White Ν 笮 基> N th butyl 2 mono-C 3 monoamino-2 — gas — 5 mono (phenyl) mono 2 9 3 * 4 9 5 tetrahydromono 1 Η mono (1) benzodiazepine-1 monoyl] acetamide acetate 1 Μ • P • 2 3 9-2 4 3 V »6 8% yield 〇1 Η-NMR (δ, CDC 1 L 3) • • 1 ♦ 3 2 (s» 9 Η) f 2 • 9 8 ( mt 2 Η) t 3 • 2 2 (A Β Q * JA = 1 6 9 δ ν = 2 〇4) 9 2 Η) 9 4 • 2 7 (A Β Q f J Λ Β-= 17, Δ, = 6].) $ 2 Η) 9 4. 3 1 L ( m, 1 Η), 5. 26 (m, 1 Η), 6. 8-7.6 (please read the precautions on the back before filling in this page) 丨 Installation and ordering 'This paper size is applicable to the Chinese National Standard (CNS ) A4 specifications (210 X 297 mm) -149 A6 B6 Printed by the Central Bureau of Standards, Ministry of Economic Affairs, S Industry and Consumer Cooperatives V. Invention Instructions (147) (m 9 1 4 Η) t 7 • 7 9 (bsf 1 Η) 〇1 3 C Ν Μ R (δ »CDC 1 3): 28.6, 3 7 • 7 &gt; 4 4 • 4» 4 7 • 7 4 9 ♦ 4% 5 3 • 5 »5 8 • 5» 1 1 7 • 1 t 1 2 1 • 5, 1 2 5 • 5% 1 2 5 • 7 t 1 2 6 • 1 9 1 2 6 • 2 1 1 2 6 • 3 9 1 2 7 • 0 9 1 2 7 • 6 »1 2 7 • 7» 1 2 7 • 9 9 1 2 8 • 7 »1 2 8 • 8 f 1 2 8 • 9» 1 2 9 • 2 t 1 3 0 ♦ 2 t 1 3 3 • 8 »1 3 8 • 1 &gt; 1 3 9 • 2 • 1 4 0 • 9, 1 4 1 • 4, 1 4 2 • 2 1 5 4« 8 &gt; 1 6 8 • 1 t 1 7 3 • 5 0 IR (cm -1 9 κ B Γ) • 1 6 5 0 wide (C = 0) 〇FAB Μ s (%) • 6 0 9 (parent + 1 • 8) »4 4 6 (5 6) 1 2 9 3 (3 7) &gt; 2 2 0 (5 7) 9 1 9 4 (4 4) 9 9 1 (1 0 0) ο Analysis and calculation C 3 6 Η 3 7 Ν 4 0 3 C 1 • C 7 0 • 9 8 t Η 6 • 1 2 1 Ν 9 • 2 〇0 experiment • C 7 0 • 6 8 9 Η 6 «3 0 t Ν 8 • 9 5 〇 Yu Shi 7 N-benzylamine • third Dinghua 2-i 3 (3 (3 methoxy Benhua) Gland Hua) 2 Oxygen (5 (Benzhua) 3 4 5 Tetraoxy 1 Η (1) Benzene φ m Miscellaneous leather 1 Hua] Acetamide as in Example 1 White Ν Benzyl t Ν __ Third butyl 2 — C 3 —- Amino one 2-Gas one 5-(phenyl) _2, 3, 4, 5-tetrahydro one (please read the precautions on the back before writing the clothing page) This paper size is suitable for China Standard (CNS) A4 specifications (210 X 297 mm) -150 2139G1 A6 B6 V. Description of the invention (148) 1H— (1) Benzazazepine-1 1-yl] acetaminophen acetate, Μ.P. 222 — 2261C, 62% yield. ^ -NMR (δ, CDC13): 1.33 (s, the Ministry of Economic Affairs Central Standards Bureau employee consumer cooperation du printing 9 Η) t 2 • 9 0 (mt 1 H) 9 3 • 0 9 (m 9 1 H 9 3 1 7 (ABQ f J Λ 0 =: L 6, △, = 2 3 6) t 2 Η) t 3 ♦ 6 5 (s 9 3 H) 9 4 • 1 — 4 • 3 (m 3 Η) 9 4 • 7 7 (mt 1 H) i 6 • 4-7 • 4 (m 1 4 Η) t 7 ♦ 5 5 (bs »1 H) 〇13 c — NMR (δ» CDC 1 3): 28.5, 3 7 * 9 $ 4 4 • 4 f 4 7 • 7, 4 9 • 4 »5 3 • 3 5 5 * 1 t 5 8 • 3 $ 1 0 4 • 2 9 1 0 9 • 0 f 1 1 1 • 6 f 1 2 5 • 5 t 1 2 5 • 8 t 1 2 6 • 2 9 1 2 6 • 9, 1 2 7 • 0 t 1 2 7 • 6 »1 2 7 ♦ 7 t 1 2 7 • 9 * 1 2 8 * 0 $ 1 2 8 • 6 9 1 2 8 • 8 t 1 2 9 • 1 9 1 3 0 • 2 $ 1 3 8 ♦ 3 * 1 3 9 • 2 t 1 4 0 • 8 &gt; 1 4 1 * 4 ♦ 1 4 2 • 3 &gt; 1 5 4 • 8 t 1 5 9 • 9 t 1 6 8 * 2 t 1 7 2 • 8 0 IR (cm -2 $ KB Γ) • • 1 6 5 0 width (C = 0) Μ S (%) • 6 0 5 (parent + 1 9 1 0 t 4 4 2 (7 2) $ 2 9 3 (5 5) 9 2 2 0 (5 9 ) t 1 9 4 (5 6) $ 9 1 (1 〇〇) o Analysis calculation C 3 7 H 4 0 N 4 0 4 ♦ 1 • 5 H 2 0:: C 7 0 • 3 4 f H 6 8 6 t N 8 • 8 7 〇Experiment • • c 70. 40, Η 6. 4 8, N 8.65 (please read the precautions on the back before writing this page) 丨 installed. Ordered · iquan. The paper size is suitable for China National Standard (CNS) A 4 specifications (210 X 297 mm) -151

_B6_ Fifth, the description of the invention (149) Fen Shi Example 5 8 N — the third pentyl 2- ί3- (3 — (3 — Shen phenyl) urea) a 2 — hydrogen 5 — (seal) a 2. 3. 4. 5 — Tetra-1 1 Η — (1) Rongxenoxenia leather 1 1 1 acetone tyramine is prepared in Example 1 from N — third pentyl 2 — [3- —amino 1 2 — Gas 5 — (phenyl) — 2, 3, 4, 5 — tetrahydro-1H— (1) benzodiazepine-1 1-yl] acetamide acetate, M. Ρ. 226 — 229C, 70% production rate. ^ -NMR (δ, CDCl ^): 0. 73 (t, J (Please read the precautions on the back before writing this page) Printed by the Consumer Labor Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs = 7 t 3 Η) t 1 • 2 1 (sf 9 H) f 1 • 6 3 (qf J = 7 »2 Η) 2 * 2 3 (s% 3 H)» 2 * 8 8 (m »1 Η) t 3» 0 4 (m »1 H)» 3 • 2 6 (AB q, JAB = 1 6 f Δ V = 2 8 2) »2 H)» 4 • 1 1 (m 9 1 Η) 9 4 • 6 0 (m »1 H ) »5« 8 0 (bs 9 1 H) »6 • 5 — 7 • 4 (mt 1 3 H)» 7 • 7 0 (b S 9 1 Η) Ο 13 c — Ν MR (δ »CDC 1 3 ) * i: 8. 3, 2 1 • 4, 2 6 * 2 9 3 2 • 8 t 3 7 • 1 f 4 4 • 4 9 5 0 • 2 f 5 3 • 6 9 5 4 • 4 t 1 1 6 • 7 9 1 2 0 • 4 I 1 2 0 * 5 $ 1 2 3 • 5 »1 2 4 • 8 t 1 2 6 ♦ 3 f 1 2 6 ♦ 5 f 1 2 7 • 7 •» 1 2 8 • 3 t 1 2 8 • 6 t 1 2 9 • 0 * 1 3 0 • 8 »1 3 8 * 3 &gt; 1 3 8 ♦ 7 f 1 3 9 • 1 f 1 4 1 • 2 9 1 4 1 • 8 t The size of this paper is in accordance with Chinese National Standard (CNS) Grade 4 (210 X 297 mm) -1 52 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 1; 9G1 A6 '_B6_ V. Description of the invention (150) 155.4, 167.5, 173.0. IR (cm'1, KBr): 1650 寛 (C = 0) 0 FAB MS (96): 513 (parent +1, 65), 426 (50), 119 (100), 103 (48) 〇Analysis calculation C η Η 3βΝ 4〇3: C 7 2. 6 3, H 7. 0 8, N 10. 93. Experiments: C 7 2. 5 7, H 6. 7 8, N 10.67. Example 5 9 N—Third-pentyl 2-f3- (3- (3-—Rongmou) ureido) —2-gas —5 — (Studyl) —2. 3. 4. 5 —Tetraargon-1H— (1) Juyou Xenonyl-1—1] 7 · Dioxamide according to Example 1, prepared from N —Third Group 2-[3 -amino group 2-oxo 5-(phenyl)-2, 3, 4, 5-tetrahydro-1H-(1) benzodiazepine-1-yl] acetamide acetate, Μ.P. 219 — 222¾, 73% yield. iH-NMR (δ, CDCla): 0.74 (t, J = 7, 3 H), 1. 23 (s, 9 H), 1. 64 (q, J = 7, 2 H) 2. 9 4 (m, 1 H), 3. 01 (m, 1H), 3. 32 (AB ,, J ab = 1 6, Δ, = 274, 2 H), 4. 15 (m, 1 H), 4. 59 (m, 1 H), 5. 73 (bs, 1 H), 6. 5-7. 4 (m, 1 2 H), 7. 57 (bs, 1 H), 7. 97 (bs, 1 H) 〇 (please read the notes on the back ^ item first and then fill in this page) — Binding · Order ·-^-This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -153 A6 B6 Economy Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry V. Invention Description (151) i3C-NMR (δ, CDCla): 8. 4, 26. 2, 32. 9, 36. 9, 44. 5, 50. 4, 53.2 , 54.7, 1 1 7. 0, 118.9, 119.0, 122. 1, 124. 3, 124. 4, 126.3, 126.4, 1 2 6. 6, 127.8, 128.3, 1 2 9. 1, 1 2 9. 5 , 130.9, 134.3, 1 3 8. 2, 140.7, 141. 1, 1 4 1. 8, 1 5 5. 1, 167.2, 173.2. IR (cm—, KBr): 1650 wide (C = 0) 〇FAB MS (96): 533/535 (parent +1, C135 / C13734 / 13), 446 (75), 293 (60), 2 2 0 (8 6), 1 9 4 (1 0 0) 〇 Analysis and calculation of C 33N 4〇3C 1: C 6 7. 6 0, H 6. 2 4, N 10. 26. Experiments: C 6 7. 2 5, H 6. 0 6, N 10.27. Fenshi Example 6 0 Reverse 1- (箆 三 丁某 acetamide) —3 — (3 —Shenzhu ureido group) —5.7.—Dijuki six-gas mixture leather 1—Brew A 2 . 4 — Er Mo ring was prepared according to the method of Hussey. AS and Herr. R.R.. J. Org. Chen .. 24, 843 (1959), in a 5 0 0 mi? Circle equipped with 1 ^ 2 entrance Add 37g (0.212mB〇l) to the bottom flask (please read the precautions on the back before filling in this page) This paper size is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm> -154 21 · ice i A6 B6 Printed by the Central Bureau of Standards of the Ministry of Economic Affairs. Printed by Thorium Consumption Cooperation V. Description of Invention (152) 4-Phenylcyclohexanone and 80m of tetrachloride. Add 30ml to the stirring solution dropwise in l〇mi ? 4. 5mJ? (0. 255 mol) sulfonamide atmosphere solution in the four gasification. This solution was stirred at room temperature for 14 hours and poured into a saturated aqueous solution of hydrogen sulfonate. The organic phase was separated, and then hydrogen acid Washed with a saturated aqueous solution of sodium, dried with sodium sulfate, and evaporated to a yellow oil, 34.8 g (78%), which was used directly in the next step. 2H — NMR (δ, CDC13): (mixture of diastereomers ), 1. 9 a 3. 6 (continuous multi-line, 7H) , 4.7 and 5.3 (multiple lines, 1H), 7. 2-7.4 (m, 5H) Ο IR (cm, KBr): 1 7 3 5 (C = Ο) 〇MS (96): 208/210 (Parent, Cl35 / Cl37, 36/12), 145 (49), 117 (88), 115 (83), 104 (100), 101 (88), 91 (82), 55 (67) 0 this oil Solution 40〇1〇) 2 benzene and was added dropwise in 40 minutes in 83m5 (250 · · 〇1) 3.0M in ether ether solution of 3.0M phenyl magnesium bromide, cooled so that the temperature is not higher than 01. The reaction was then warmed and heated under reflux for 14 hours. After cooling, it was quenched with aqueous ammonium chloride solution, washed with water and brine, dried over sodium sulfate, and evaporated. The output is 53.9 g (about the theoretical value), and the unprocessed oil is directly used in the next step. ^ -NMR (δ, CDCla): (mixture of diastereomers) 1. 9-3. 3 (twinned multiple lines, 7H), 3. 9 (m, lH), 7.1-7.6 (m, 10H) 〇The standard of this paper is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 «Centimeters) ~ 155 (please read the note item first and then fill in the clothes to buy)-install and order. 213901 A6 B6 V. Invention Description (153) B. 2.4—Dijury hexamidine_oxime The above oil was dissolved in 200 mi of methanol, and added 18. 6 g (0. 267 «〇1) of hydroxylamine hydrochloride and 37.2 mi? (Ο. 267« ι〇1 ) A solution of triethylamine in ΙΟΟιηβ formazan. The solution was poured to separate the oily precipitate and stirred at room temperature for 1.5 hours. The white precipitate was filtered and dried to produce 13.6g (31%) of a white solid, mp214 — 215 ^ 0 C · 5.7-dironyl six-gas xenon mixed leather 2 —_ 25〇mi equipped with N2 inlet? 8.52 g (32.1 5 inmol) 2,4-diphenylcyclohexanone and 1 10 mi pyridine were added to the round bottom flask. Once the solids are dissolved, the solution is cooled to 〇υ, and 12.3g (64.3 mmol) p-toluenesulfonaldehyde gas is added. The reaction was stirred for 16 hours while melting in an ice bath and the reaction was allowed to warm to room temperature. It was then poured into 300 mj? 3 N HCi, extracted into ethyl acetate, and the organic layer was washed with additional HCI and brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel, using methanol / dichloromethane as the eluent, to produce 2. 4 8 (28%) oil printed by the Xingong Consumer Cooperative of the Central Bureau of Economics of the Ministry of Economic Affairs, which was produced by crystallization of isopropanol. P 1 7 1-17 3. 5 t: O 1 Η--NMR (&lt; 5, CDC 1 3): 2.0 (m, 1 H), 2 1 (m, 3 H), 2.7 5 (m, 2 H), 2.9 5 (m, 1 H), 4.60 (m, 1 H) 9 5 .7 8 (bs, NH, 1 H), 7.1-7.5 (m, (Please read the precautions on the back first and then this page) Applicable to the size of clothing paper (CNS> A4 specifications (210 X 297 public completion) -156 213901 A6 B6 V. Invention description (154) 1 Ο Η) 0 Printed by R Industrial and Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs 1 3 C-N MR (δ »CDC 1 3): 30.3, 3 6 • 3 $ 4 5 • 3 9 4 8 • 6 9 5 8 • 1 »1 2 6. 3 f 1 2 6 • 6, 1 2 8 • 4 f 1 2 8 * 7 $ 1 2 9 .2, 1 4 2 • 1, 1 4 6 • 1 9 1 7 6« 5 0 IR (cm -1 t Κ Β Γ) • 1 6 6 2 (c = 0) 〇 S S (%) • 2 6 5 (parent t 8 2) t 2 6 6 (85) 9 1 6 0 ( 4 7) 9 1 0 6 (1 0 0) t 1 0 4 (87) 〇 Analysis and calculation C 1 S Η 1 9 Ν 0 • C 8 1 • 4 8 * Η 7 • 2 1 9 N 5 «2 7 〇 Experiment ♦ • C 8 1 ♦ 3 2, Η 7 • 4 1 9 N 5» 2 8 0 D 3 -Bromo 5 «7 monophenyl hua radon m mixed leather -B 9 equipped with an addition funnel and N 2 into P 2 5 0 m 9. Add 1 • 5 1 g (7 * 2 7 to the bottom flask mmol) Phosphorus pentachloride and 2 5 m anhydrous digas methane 0 Cool the solution to 0 V with stirring. Add 1 • 9 3 g (7 • 2 7 mmol) 5 t 7 — 2 Phenyl IS m mixed leather one 2 one ketone and 1 • 1 8 m (1 4 • 5 mm 〇1) pyridine in a 50 m S. Nitrogen gas solution 0 reaction at 0 t: stirring for 5 minutes, then Add 0 • 8 2 m 5 (1 6 • 0 mmol) of bromine in 5 m dichloromethane dropwise in 5 minutes. Reaction at 0. Save and mix for 5 minutes $ and then at room temperature for 1 • 8 hours. Evaporation reaction taken at 4 0 m 9. 1 • • 1 Tetrahydrofuran • • Stir in water for 1 • 2 hours 0 Then pour the reaction into water and extract this paper standard is applicable to the CNS A 4 specifications (210 X 297mm) _ 157 (Please read the notes on the back before filling in this page) 2139G1 A6 B6 Printed by the R and Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Description of invention (155) in ethyl acetate. The organic layer was washed with sodium bisulfite aqueous solution and brine, dried with sodium sulfate, and evaporated to an oil. The oil was ingested in 20 mi of dichloromethane and 20 mp of ethanol, and hydrogenated at 42 ps i for 1 hour in the presence of SO. 30 g of 10% sodium rake and 3 drops of quinoline. T 2 c shows that most of the expected monobromo product R / = 0.4, there is a trace of dibromo precursor at R / = 0.7 and the aldamine in the raw material is located at R / = 0.15, at 1/1 One ethyl acetate / in the hospital. This reaction was filtered through Celite with ethanol and methane, evaporated, and chromatographed on silica gel, using 2 / 1-hexane / ethyl acetate as the eluent, to produce 2.06 g (82%) foam. Μ. P. 70-781C. ^ -NMR (δ, C Ό C \ β): (mixture of diastereomers) 1. 9 — 2. 7 (m, 4H), 3. 12 and 3. 52 (multiple lines, 1H), 4. 52 and 4. 76 (multiple lines, lH), 5.01 (m, lH), 5.79 & 5.89 (broad singlet, 1H, N Η), 7.1-7.4 (m, 1 0 Η) 〇13C-NMR (δ, CDCla): 42. 4, 44. 0, 4 8. 0, 5 0.5, 57. 6, 1 2 6. 3, 1 2 6. 6, 1 2 6. 9, 1 2 7. 1, 1 2 8. 7, 128.9, 1 2 9. 3, 1 2 9. 4, 169.6. IR (cm'2, KBr): 1667 (C = 0) 〇MS (96): 343/345 (1 1/10, parent Br7e / 8i), 236 (32), 117 (32), (please first Read the note $ item and $ clothing page on the back) This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -158 A6 B6 213901 V. Invention description (156) 106 (100), 91 (39), 55 (31) 〇Analysis and calculation of C! 8Hi8NOBr: C 6 2. 8 0, Η 5. 2 7, Ν 4. 07. Experiment: C 62. 86, Η 5. 2 6, Ν 3.98. Ε. 1 one (third butyl ethyl amine) one 3-submerged one FS. 7-Errong a six gas argon heterogener one 2 equipped with a liquid addition funnel and 1 ^ 2 inlet 1 OOmi 3-neck round bottom 0.32 g (6.59 mmol) of sodium hydride was added to the flask, and then washed with hexane and 4m β anhydrous tetrahydrofuran. To this stirred suspension was added 2. 06g (5. 99 mmol) 3 mono-_5, Ύ-diphenyl hexahydroazazepine-2-one and 1. 59g (6.5 9 mmo 1) third butyl A solution of acetyl iodide. The reaction was stirred at room temperature for 60 hours, quenched with ammonium chloride solution, then poured into water, extracted twice with ethyl acetate, washed with brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel using 2 / 1-hexane / ethyl acetate as the eluent, producing 1.585 g (58%) oil, R / = 〇 · 4 (1 / 1-hexane / acetic acid Ethyl)

^ H — NMR (δ, CDCla): (mixture of diastereomers) 1. 22 and 1. 25 (single peak, 9H, ratio 35/65), 2. 0-2 · 7 (m, 4H ), 3. 08 and 3.21 (multiple lines, 1H), 3. 5-3. 9 (m, 2H), 5. 01 and 5. 4 -5.7 (m, 2H), 7.1-7. 4 (m, 1 0 Η) 〇 (please read the notes on the back and then f buy) 丨 Package · Order · Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. The paper size is in accordance with the Chinese National Standard (CNS) A 4 specifications (210 X 297 Public) -159 丄 A6 B6 V. Description of the invention (157) i3C-N MR (δ 9 CDC 1 3): 1 4. 2, 2 6 .9 2 8 • 7 9 4 0 • 6 t 4 3. 9 »5 1 ♦ 1, 6 0 .3» 6 1 • 7 »1 2 6 • 8 t 12 7« 0 &gt; 1 2 8. 2 9 1 2 8 • 4 f 1 2 8 • 7, 1 2 8 • 9 $ 1 3 9. 5 t 1 4 4 • 6 9 1 6 7 • 5, 1 7 0 • 0 〇IR (C m -1 9 Κ B Γ) • 1 6 7 5 and 1 6 3 2 (C = 0) 0 MS (%) ♦ • 3 7 7 (Parent — B Γ, 3 9) »3 0 4 (4 2) 9 2 1 9 (2 1) 9 1 4 4 (2 5), 1 1 8 (3 1), 1 1 7 (3 3), 1 1 5 (4 2) »1 0 4 (2 1) , 9 1 (1 0 0), 5 7 (5 0) 9 5 5 (34>. F. 1 (The third butyl huazt amide) 3 — Matrine fluoride 5 «7-Diphenyl hexahexaazatriazine leather One-one ketone filled with N 2 into P is added to a 100 m round-bottom flask. 1 • 5 8 g (3.46 mmol) 1 mono (third butyl ethylpyramine) mono 3 monobromo-5 1 7 -Diphenyl hydrazine leather-2-ketone, 5 m anhydrous dimethylformamide, and 0 • 2 7 g (4 • 1 5 mm 〇1) superimposed sodium 0 reaction at 8 0 V heating 3 «5 days, cooling 9 Pour into water and extract in acetic acid (please note # item before f to buy this)-install-order.-Central Ministry of Economic Affairs wrx. Consumer Cooperative Printed« ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel, using 40% ethyl acetate in hexane as the eluent, to produce 1.09 g (75%) of oil, which was found to be an 8/3 diastereoisomeric mixture, R / = 〇. 4 — 〇. 5, in 1/1 monoethyl acetate / hexane. This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -160 Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 213901 A6 ____B6_ V. Description of the invention (158) 'H-NMR (δ, CDCla ): 1. 21 and 1.31 (single peak, 9H), 2. 17 and 2. 58 (multiple line, 4H), 3. 05 and 3.32 (multiple line, 1H), 3. 57 (AB «, Δ „= 213 2 one of the proton information isomers CH. CONHt-butyl), 4. 4-5. 0 (multiple lines, 2H), 5. 68 and 6. 17 (single peak, 1 H, li H) , 7.〇-7.3 (m, l〇H) 〇IR (cm ^, KBr): 2 1 0 5 (N 3), 1 6 4 7 (C = 0) 〇MS (%): 377 (parent —N3, &lt;; l), 319 (Parent one (CONHt-butyl), 4), 235 (21), 1 4 6 (4 3), 1 15 (47), 104 (73), 103 ( 40), 91 (100), 84 (32), 57 (46) o G · 1 one (third butyl ethyl sleep amine) one p _ 5. 7 — Errong a six gas qi Zaza 1 2__ 1 . 0 9 (2 · 6 0bib〇1) 1- (third butylacetaldehyde amine)-3- azide-5, 7-diphenyl hexahydrogen leather 2- 2-one in 30 m ethyl alcohol Solution and 15m)? Dichloromethane was hydrogenated with 42 ps i hydrogen for 36 hours in the presence of 0.40 g of 10% aluminum rake. The alcohol and methane are filtered through Celite, evaporated, and chromatographed on silica gel, using 30% methanol in ethyl acetate as the eluent, which produces 300 ng (29%) of less polar diastereomers Isomer oil and 4. 20 «g (41%) oil of higher polarity diastereomers. (Please read the notes on the back before writing this page) —Package · Order 丨 This paper size is applicable China National Standard (CNS) A4 specifications (210 X 297 mm) -161 213901 A6 B6 V. Description of the invention (159) Low mixing and lack of anti-anti-M materials: Printed by Beigong Consumer Cooperatives, Central Bureau of Standards, Ministry of Economic Affairs 2H-NMR (δ, CDCla): 1. 25 (single peak, 9 Η) t 2 • 1 8 t 2 • 5 0 and 3 • 2 3 (multiple lines 9 7 H) t 4 • 5 2 and 4 • 9 0 (multiple lines 1 2 H), 6 • 5 (wide DO early peak t 1 H f N ID f 7 • 0 a 7 • 4 (mt 1 0 Η) o 1 3 C — NMR (δ &gt; CDC 1 3) «2 8. 8, 3 7 • 7 9 4 0 • 5 &gt; 5 1 • 3 &gt; 5 1 • 7 f 5 2 • 7 9 6 0 • 3 t 6 4 9 1 2 5 • 6 t 1 2 6 • 5 t 1 2 6 • 8, 1 2 7 • 8 t 1 2 8 • 7 f 1 2 9 • 1 t 1 4 0 • 7 9 1 4 5 • 4 t 1 6 7 • 9 &gt; 1 7 1 o IR (cm -2 9 KB r) »• 1 6 5 5 (c = 0) Ο Compared with the lid polar enantiomer • • 1 Η- -NMR (δ, CDC 1 1 3) 1 • 2 0 (single peak $ 9 Η) f 1 • 9 — 2 • 5 (multiple lines 9 4 H) $ 3 • 1 0 (mf 1 H) 9 3 • 5 6 (ABQ f J Λ B = L 6, Δ, 2 1 3 9 2 H) 9 4 • 1 2 (df J = 1 6 t 1 Η) t 4 # 9 9 (d »J = 1 0» 1 H ) f 5 * 6 8 (broad singlet t 1 Η »N HJ &gt; 7 • 1 — 7 • 4 (m» 1 0 H) Ο 1 3 C-NMR (δ t CDC 1 3) 4 4:28. 6, 3 9 • 4 9 4 1 • 8 t 4 6 • 6 &gt; 4 8 * 3 9 5 0 • 8 9 5 3 • 2 1 6 0 • 7 »1 2 6 • 7 t 1 2 6 • 8, 1 2 8 • 5 f 1 2 8 • 6 &gt; 1 2 8 »8, 1 2 9 • 5 t 1 3 8 • 4 f 1 4 5 • 5 f 1 6 8 • 0 9 1 7 7 • 4 〇 ( Please read the precautions first and then fill out this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -162 213901 A6 B6 V. Invention description (160) IR (cm_i, KBr) : 1645 and 1670 (shoulder) (C = 0) 〇MS (96): 393 (parent, 1.4), 265 (17), 193 (24), 132 (100), 91 (27). Η. Anti-one 1 one (the third butyl acetamide) one _3 — (3 — toluene a certain urea) one 5.7 — dironyl six gas xenon mixed leather one 2 — 35mi equipped with Ν2 inlet ? Round bottom flask was added 150 (Ο.382〇ιβ〇1) 1-(third butylacetaldehyde amine)-3-amino one 5, 7-diphenyl hexahydroazazepine-2-ketone (Lower diastereoisomers), 4mi 1,2-dichloroethylate • and 49mi? (0.38 2 »im〇l) 3-tolyl isocyanate. The reaction was stirred at room temperature for 2.7 hours, diluted with 10 volumes of diisopropyl ether, stirred for 30 minutes, filtered, washed with diisopropyl ether, and dried to a white solid, Μ.P. 245-246 ^, 1 〇9 nick (54%) 〇2H-NMR (δ, CDC13): 1. 26 (Single peak, (please read the notes on the back before writing this page) • Binding · Order. R Engineering, Central Bureau of Standards, Ministry of Economic Affairs Printed by consumer cooperatives

9 Η) &gt; 1. 7 one 2 «6 (multi-line $ 5 Η), 2 • 2 3 (S» 3 Η), 3 • 6 4 (m 9 1 Η) t 3 • 8 0 (AB, » JAB — 16 f Δ V = 3 9 9 f 2 Η) 9 4 • 1 4 and 4 • 6 — 4.8 (multiline 9 2 Η) »6» 5 7 (d J = 9 &gt; 1 Η), 6 • 7 0 (df J =: 7 f 1 Η) f 7 • 0 — 7 • 6 (m, 1 0 Η) t 8 • 8 3 (broad singlet f 1 H) o IR (cm'1, KBr ): 1673 and 1640 (C This paper standard is applicable to China Home Standard (CNS) A4 specifications (210X297 mm) 213901 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (161) = 0) 〇 MS (96): 526 (parent, &lt; 1), 235 (73), 2 3 4 (8 2), 1 9 3 (36), 1 3 2 (1 0 0), 57 (32), 43 (46), 41 (32). Analysis and calculation C32H38N4〇3 · 1.75H2〇: C 68.86, Η 7.49, Ν 10.04. Experiment: C 68. 90, Η 7. 2 5, Ν 9.86. Fen Shi Example 6 1 Bianyiyiyi (the third butyl 7 "amide) 3-(3_ 申 氲 荣 某 脤 某)-5. 7-diphenyl six gas mixed leather-2-Si made from Example 6 Diastereomer of a lower polar amine of 0 G, 49% yield, mp 242-244t: 〇iH — NMR (δ, CDC13): 1. 26 (single peak, 9H), 1. 7 — 2. 6 (multiple lines, 5H), 3. 64 (m, 1 Η), 3. 69 (s, 3 Η), 3. 81 (A Β,, Jn = 16, = 401, 2Η), 4. 14 and 4. 6 — 4. 8 (multiple lines, 2Η), 6. 6 — 6. 9 (multiple lines, 2Η), 7. 0 — 7. 6 (m, 10Η), 8. 34 (wide Single peak, 1H). IR (cm-, KBr): 1673 and 1640 (C = 0) MS (96): 542 (parent, 0.9), 348 (16), 3 0 5 (6 8), 2 3 5 (5 8), 2 3 4 (This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -164 (please read the precautions on the back before filling out this page) 丨 Installation- Ordering_Ministry of Economic Affairs Printed by the Staff Consumer Cooperative of the Bureau of Standards 213901 A6 _B6 V. Description of invention (162) 65), 149 (1 0 0), 132 (8 9), 123 (33), 91 (39), 57 (39), 44 ( 47) 〇Analysis and calculation of C32H38N4〇4 · 1. 5H2〇: C 67. 47, Η 7. 25, Ν 9.83. Experiment: C 67.52, Η 7.17, Ν 9.60. Example 6 2 Shunyi 1-1 (t-butyl acetamide) 3 — (3-methylbenzyl ureido) — 5. 7 — Diphenyl hexafluoroethylene mixed leather 2 —_ Made from example 60G Highly polar amine diastereomer, 68% yield, M.P. 253-253. 5t: 〇2H-NMR (δ, CDC13): 1.15 (single peak, 9H), 1.9- 2. 7 (multiple line, 4H), 2. 22 (s, 3 Η), 3. 27 (m, 1 Η), 3. 50 (A Β,, Jab = 16, Δ, = 224, 2Η), 5. 09 (dd, J = 1, 5, 1 Η), 5. 29 (d, J = 1 0, 1 Η), 6.69 (d, J = 7, 1H), 6.83 (d, J = 6, 1H), 7.0-7.6 (m, 11H) 〇IR (cm-, KBr): 1660 (width, C = 0) o MS (%): 526 (parent, 0.8), 320 (32), 319 (3 8), 2 3 5 (4 4), 2 3 4 (44), 133 (1 0 0), 132 (9 1), 57 (41), 4 4 (36), 41 (38), 39 (33 ). Analysis and calculation C32H38N4〇3: C 72. 98, Η (Please read the precautions on the back before filling out this page) This paper size is applicable to the national standard (CNS> A 4 specifications (210 X 297 mm) -165 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of Invention (163) 7. 2 7, N 10. 64. Experiment: C 72. 94, Η 7. 31, Ν 10.45. Fen Shi Example 6 3 1 A (the third butyl acetamide) a 3- (3-methyl urethane urea) a 5.7-diphenyl six gas mixed leather a 2-Gu I from the example of the 60G higher polar amine Diastereomer, 43% yield, mp 1 66-1 73 ^ 0 iH-NMR (δ, CDC13): 1.15 (single peak, 9H), 1.9—2.7 (multiple lines, 4H), 3. 25 (m, 1H), 3. 52 (AB «, Jab == 1 6, = 225, 2 H), 3. 69 (s, 3 H), 5. 09 (m, 1 H), 5. 29 (d, J = 1 0, 1 H), 6. 45 (d, J = 8, 1H), 6.84ls, 1H), 7.0-7.6 (m, 1H) 〇IR (cm ^ , KBr): 1645 (wide, C = 0) o MS (96): 542 (parent, &lt; 1), 265 (15), 2 3 5 (3 7), 2 3 4 (3 4 0), 193 (18), 149 (100), 123 (15), 91 (41), 78 (18), 57 (16) 0 Analysis and calculation C32H3SN4〇4: C 70.83 , H 7. 0 6, N 10. 32. Experiment: C 7 0. 6 6, H 6. 8 0, N 10. 3 2 〇 The paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) 166 (please read the back (Note ί item and fill in this page) 21 A6 B6 V. Description of the invention (164) Example 6 4 1 1 (third butyl acetamide) 3 — (3 — gas urea) —5 · 7 -Dibenzyl six-gas mixed leather one 2-touched from the higher polar amine diastereomer of Example 60G, 36% yield &gt; Μ • Ρ • 7 8-1 8 5 X: O 1 Η --Ν Μ R (δ, CDC 1 3) 1. 1 5 (single peak f 9 Η) »1 • 9 — 2 • 7 (multiple entry, 4 Η) &gt; 3 • 2 7 (m» 1 Η ) &gt; 3 • 5 1 (AB 9 t J ^ Β = 1 6, Δ „2 2 6 &gt; 2 Η) 5 • 0 9 (dd 9 J = 1 9 5» 1 Η) »5 • 2 9 ( d »J = 1 0 t 1 Η) 6.9 — 7 • 5 (mt 1 2 Η)» 7 «6 8 (s 9 1 Η) ο IR (C m -1 1 KB r) • 1 6 6 5 And 1 6 4 2 (drag at 1 6 8 2) (C = 0) o M S (%): 5 4 6/5 4 8 (parent, c 1 3 5/3 7 »&lt; 1) f 2 6 5 (1 4 ) &gt; 1 9 3 (2 1) f 1 5 3/1 5 5 (1 0 0/3 4 »C 1 3 5/3 7) f 1 1 .5 (2: L) 9 9 1 (2 8 ) 9 9 0 (2 5) t 5 8 (2 9) 〇 Analysis calculation C 3 1 Η 3 5 N 4 0 3 C 1 • C 6 8 • 0 6 »H 6 • 4 5 &gt; Ν 1 0 • 2 4 〇Experiment • C 6 7 • 7 3 t H 6 • 1 3 t Ν 1 0 • 0 7 o H R M S Calculate C 3 1 H 3 5 N 4 0 3 C 1 3 5 · 546. 23895. Experiment: 546. 23581 Printed by Beigong Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs -167 (please read the precautions on the back before filling in this page) This paper size is applicable to China National Standard (CNS) Grade 4 (210 X 297 mm ) Example 6 5 A6 B6 Printed by the Central Standards Bureau of the Ministry of Economic Affairs, Industry and Consumer Cooperatives of the Fifth, Invention Instructions (165) 1 One (Second T huanamide) One 3 One (3 — Benzene M Hua) 5 7 One Diphenyl hua_JL_ * Hydrogen mixed leather 2 Preparation example 6 Higher polar amine diastereomers of 0 G »4 6% yield f Μ • P. 2 3 3 — 2 3 4 VO 1 Η- -NMR (δ, CD 3 s 0 CD 3): 1.. Ί 4 (t $ J = 7, 3 H) &gt; 1 • 1 5 (ao early peak t 9 H) ί 1 • 8 — 2 • 1 (m »3 Η)» 2 • 4 9 (m 2 H) 9 2 • 5 1 2 • 7 (m 9 1 Η) t 3 • 2 3 (m 9 1 H) 9 3 • 5 1 (ABQ t J ^ B =: L 6, △, = 2 2 5, 2 Η) t 5 • 0 7 (m 9 1 Η) 9 5 • 2 8 (d 1 J = 1 0 $ 1 Η) 9 6. 7 2 ( dt J = 8 9 1 H) »6 • 8 2 (d 9 J = 5, 1 H) 9 7 * 0 — 7 • 6 (m 9 1 4 Η) 9 8 • 9 4 (bs ， 1 Η) 13 Η -NMR (δ fc D 3 S 0 CD 3) • 1 5 • 6 t 2 2 • 8, 2 8 * 5 4 5 • 0 f 4 7 • 0 t 4 9 • 9 f 5 1 • 5, 5 9 «4 f 1 2 0 * 6 9 1 2 6 • 8 I 1 2 8 • 5, 1 2 9 • 4 &gt; 1 3 9 • 2» 1 4 0 ♦ 5 $ 1 4 4 • 2, 1 4 6 • 3 &gt; 1 5 4 • 1 »1 6 7 • 3 9 1 7 3 • 3 〇IR (cm -i $ Κ B Γ) • 1 6 6 0 ( Width f C = 0) 〇 S (96) • • 5 4 0 (Parent $ 2) t 3 2 3 5 (2 1), 147 (32), 132 (100), 121 (48 (please read first (Notes on the back will be written on this page).

-II This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm)-168 7 2. 1 0, Η 7. 5 2, N 10 .1 9. Experiment: C 7 2. 1 5 , Η 7. 1 6, N 9. 7 4 (-0. 4 5 / Ο A6 ^ _ V. Description of the invention (166)), 91 (31) 〇 analysis calculation C33H4〇N4〇3 1/2 Η2〇: C Fenyu example ft 6 1 one (ditributyl acetamide) 3-(3-trifluoromethylphenylureido)-5. 7-two Zhu six six krypton mixed leather-2- ketone system Since the case of 60G higher polar amine diastereomer, 36% production (please read the precautions on the back and then fill out this page) i equipment · Print rate t M • P • Employee Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs 2 6 3-2 6 4 υ 〇2 H--NMR (δ, CD 3 s 0 CD 3) 4] 1 5 (single peak 9 9 H) &gt; 1 • 8 — 2 • 1 (m • 3 H) * 2 • 5 8 (m 9 1 H) »3 • 2 3 (mt 1 H) f 3 • 5 1 (ABQ 9 J λ B: = 1.6, Δ, = 2 2 7, 2 H) f 5 . 1 0 (dd 1 J = 1 t 5 t 1 H) t 5 • 3 0 (dt J = 1 0 9 1 H) 9 6 • 9 5 (d &gt; J = 5 9 1 H) 9 7 • 0 2 (s »1 H) t 7 • 1 — 7 • 5 (mt 1 3 H) t 8 • 0 0 (bs 9 1 H) »9 • 4 1 (bst 1 H) 〇13 H — NMR (δ 9 CD a S 0 CD 3) • 2 8 • 5 f 4 4 • 9 t 4 7 • 0 $ 5 0 • 0 $ 5 1 • 6 t 5 9 • 4 9 1 2 6 • 3 9 1 2 6 • 8 9 1 2 8 • 1 f 1 2 8 • 4 » 1 2 8 • 5 9 1 2 9 • 4 t 1 2 9 • 8 9 1 3 9 • 2 9 1 4 1 * 3, 1 4 6 • 2% 1 5 4 • 0 »1 6 7 2 &gt; • 17 .Λ. This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -169 A6 B6

9 Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs-X V. Description of Invention (167) 17 3. 1 〇IR (C m -2 t Κ Β r) • • 1 6 6 0 (Wide, C 0) 〇 Μ S (%) • 5 8 0 (parent t 5) »2 6 2 (5 0) &gt; 1 9 3 (6 2) t 1 8 7 (6 5) * 1 3 2 (1 0 0) t 9 1 (8 7) 9 5 7 (9 9) 〇Analysis calculation C 3 3 H 3 5 Ν 4 0 3 F 3 * • 1 L / 2 H 2 0 • C 6 5 * 1 8, Η 6 • 1 5 , N 9 climbing 50 0 〇 experiment • • c 6 2 • 2 5, Η 5 • 9 3, N 9 • 1 8 〇rwttmt Example 6 7 1 .- (third τ huanamide)-3 (3 (Methionine Benzaloxin) 5, 7 Diphenyl cap-JL · * Argon leather 2 ketone white example 6 Higher polar amine diastereomer of 0 G 9 4 9 96 Yield 9 Μ • Ρ. 1 7 0 — 1 7 6 V 0 2 Η--Ν Μ R (δ, CD 3 s 0 CD 3):] L.] Ί 5 (single peak t 9 Η) 9 1 • 9 — 2. 1 (mt 3 H) &gt; 2 4 1 (S &gt; 3 Η) t 2 * 6 2 (m 9 1 H) »3 • 2 7 (m, 1 Η)» 3.5 2 (AB &lt; 7, JAB =: L 6, Δ, = 2 2 6 »2 Η), 5 • 1 1 (dd, J = 1 9 5» 1 Η) &gt; 5 • 3 0 (d 9 J = 1 0, 1 H) t 6 • 7 7 (dt J = 5 $ 1 Η), 6 «8 5 (d, J = 5» 1 H) 7 • 〇- 7 6 (m, 1 4 Η) 9 9. 0 6 (b S t 1 Η) Ο 3H-NMR (δ, CD3SOCD3): 14.6, (please read the precautions on the back before filling in this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm)- 170 2 m A6 B6 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy V. Invention Instructions (168) 28. 5, 4 4. 9, 4 7. 0, 49. 9, 51. 5, 59.4, 114.0, 114.4, 118.5, 126.3, 126.8, 126.9, 128.5, 128.6, 129. 2, 129. 4, 1 3 8. 5, 1 3 9. 2, 1 4 1. 1, 146.2, 1 5 4. 0, 1 6 7. 3, 1 7 3. 2 〇IR (cm-, KBr): 1660 (width, C = 0) ο FAB MS (96): 559 (parent +1, 10), 3 9 4 (1 2), 2 3 3 (1 3), 193 (1 4), 155 (9 7), 1 3 5 (2 4), 119 (1 0 0), 1 0 3 (3 8) 〇Analysis and calculation C32H38N4〇3S: C 68 . 79, Η 6.85, Ν 10. 03. Experiment: C 68. 91, Η 6. 9 4 8, Ν 9.96. Fen Shi Example 6 8 1 one (the third butyl acetamide) a 3 — (3 — amide amide a certain ureido group) a 5.7-diphenyl six gas M 2 leather-2- ketone self The higher polar amine diastereomer of 60G, 18% yield, M.P. 155-16510. ; H — NMR (5, CDC13): 1.145 (single peak, 9 Η), 2. 00 (m, 1 Η), 2. 2-2. 5 (m, 3 Η), 3. 32 (m , 1Η), 3. 66 (ΑΒ ,, (Please read the precautions on the back before writing this page) This paper scale is applicable to the Chinese National Standard (CNS> A 4 specifications (210 X 297 mm) -171 21H9G1 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of Invention (169) JAB = 1 6 »Δ V = 7 3 f 2 H) t 5 • 2 5 (bs% 2 Η)» 5 • 2 8 (m 9 1 H) $ 5 • 7 6 (mf 1 H% 7 • 1 — 7 ♦ 4 (m ， 1 3 H) 9 7 • 6 7 (d $ J 7 t 1 Η) »7 • 8 0 (st 1 H ) * 8 • 1 8 (bs 1 Η) »9 • 0 9 (bsf 1 H) 0 1 3 Η — Ν Μ R (δ» CDC 1 3) 2 8. 6, 3 8 • 0 t 3 9 • 2 t 4 5 »7 t 4 7 • 9» 5 1 • 4 5 6 • 7 9 6 1 • 0 t 1 1 2 • 7 f 1 1 8 • 4 t 1 2 6 • 6 »1 2 6 * 8 &gt; 1 2 7 • 0 9 1 2 8 • 1 t 1 2 8 • 2 1 2 8 • 3 &gt; 1 2 8 • 5 &gt; 1 2 8 • 6 y 1 2 8 • 7 1 2 8 • 8 f 1 2 9 ♦ 0 »1 2 9 • 4 &gt; 1 2 9 • 5» 1 2 9 6 t 1 2 9 • 7 9 1 3 7 • 8 $ 1 3 9 • 3 »1 4 5« 0 f 1 6 7 • 0 9 1 7 4 • 8 9 1 7 9 • 9 ο IR (C m -1 »K Β Γ) • 1 6 6 0 (width tc = 0 〇FA Β Μ S (%) • • 5 5 5 (parent t 6 2) $ 4 8 1 (1 5)» 4 2 4 (2 3 ) 9 1 9 3 (5 6) »1 5 5 (2 3) 9 1 1 9 (1 0 0) t 1 0 3 (3 8) Analysis calculation C 3 2 Η 3 7 Ν 5 0 4 ♦ 1/3 H 2 O:: C 6 8 • 4 3 9 Η 6 • 7 6, N 1 2 • 4 7 0 experiment • • 6 8 • 4 7 t Η 6 4 7 t N 1 2 • 4 4 o Example 6 9 (Please read the precautions on the back before filling out this page) 丨 Installation_ Order-t This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -172 21; 19C1 A6 B6 Central Ministry of Economic Affairs Printed by the Bureau of Standards and Staff Consumer Cooperative V. -5 Description of the invention (170) 1 I (the third T ethylacetamide) 3 (4 Shen Rong certain urea) 7 芣 华 —1 ^ Hydrogen mixed leather 2 M white Example 6 The higher polar amine diastereomer of 0 G t 2 5% yield $ Μ • P • 1 5 6-1 6 5 t: o 7 Η--NMR (δ, CD 3 S 0 c D 3) • • 1 • 1 5 (BD early peak &gt; 9 H) &gt; 1 • 9 — 2 • 1 (mt 3 H) »2 • 2 0 (S t 3 H) * 2 «6 1 (mt 1 H) $ 3 • 2 7 (m, 1 Η) t 3 • 5 1 (ABQ f J Λ B = = 1 L 6, Δ, = 225 Ref 2 Η) 9 5 • 0 8 (m 9 1 H) t 5 * 2 9 (dt J = 1 0 9 1 H) &gt; 6 • 7 8 (dt J 5 t 1 Η) t 7. 0 and 7 • 2 — 7 ♦ 4 (m 9 1 5 H) f 8 • 8 7 (bs »1 Η) 0 13 Η — NMR (δ f CD 3 S 0 CD 3): 2 0 • 3, 2 8 • 5 t 4 5 * 0 t 4 7 • 0 t 4 9 • 9 t 5 1 • 5, 5 9 • 4 9 1 1 7 • 6 f 1 2 6 • 3 »1 2 6 • 8 t 1 2 8 * 5 &gt; 1 2 8 • 7 9 1 2 9 • 1 $ 1 2 9 • 2 &gt; 1 2 9 ψ 3 $ 1 2 9 • 4 »1 2 9 • 5 9 1 2 9 • 7 t 1 3 8 • 0 9 1 3 9 ♦ 3 f 1 4 6 • 3 9 1 5 4 • 2 t 1 6 7 • 3 t 1 7 3 • 4 o IR (cm -2 »KB Γ) 1 6 6 0 (width» C = 0) 〇FABMS ( %): 5 2 7 (parent + 1 9 3 0), 4 5 4 (6) »3 1 3 (1 2) 9 2 3 5 (1 0) f 1 5 7 (1 0 0) ○ Note Page Binding This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -173 t l

I I A6 B6 2139G1 V. Description of the invention (171)

Analysis and calculation C32H38N4〇3 · 2 / 3H2〇: C 71.35, Η 7.36, N 10.40. Experiment: C 71.20, Η 7. 2 6, Ν 10.23. Face Notes Example 7 Ο 1 one (Ν-the third butylacetamide) one 3-Tian Zhuji calendar one) one R. 7-two Zhu very six krypton xenon Xieza one 2-_ 鼸 analysis Bock &gt; Μ · G., Eta 1.. J. 0 rg · Chem ·, fS 2, 3232-3239 (1987) method using L-phenylalanine as the separating agent:

I page installed A · 1 — (N — third but very 7. tyramine) one 3 — — but 1 forging a certain amine) one 3 — Zhu Mou acryl makeup one 5. 7 — Errong very six Xenon hybrid economy The Ministry of Central Standards Bureau staff consumption cooperative printing

I Two leather one 2 — _ 100m (1.65 mmol) of the higher polarity isoamine with a N2 inlet) a 3-amino one 5, 7 (1.65 mmol) t — B 0 C mg (1 . 65mmol) N-by chloromethane, 317ng (1. 65 硪 化 diimine, and 0.415m. The reaction was stored at room temperature for 14 hours, the ester. The organic layer was washed with IN HC ί, and brine, Dry magnesium sulfate / 1 ethyl acetate / hexane in a round-bottomed flask with 6 5 0 «8 structure, 1 1 (third butylacetaldehyde phenyl hexahydroaza leather, 4 3 9— L-phenylalanine, 253 benzotriazole, 13mi anhydrous diethyl (dimethylamine phenyl) ί (2.98 ·· 〇1) triethylammonium was poured into water and extracted into ethyl acetate, water, Saturated aqueous solution of sodium bicarbonate and evaporated. TLC showed that the product produced R / = 0.30, and its 174 paper size is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 Gongdong) 21 * A6 B6 V 3. Description of the invention (172) is foamy, 95018 (909 ^), 0 ^ = 5.77 ° (c = 0.8, CH2CI2) 〇2H-NMR (δ, CDC13): 1.20 (single peak, 9 Η) , 1. 28 (s, 9 Η), 1. 9-2. 2 (m, 3H), 2.43 and 2.57 (of two diastereomers Heavy line, 1H), 2. 8-3. 0 (m, 3H), 3. 53 and 3. 54 (the pattern of two ABs of each diastereomer, = 15 and 15, = 198 and 195, 2H), 4.18 and 4.32 (multiple lines of two diastereomers, 1Η), 5.0 · 5.2 (m, 2Η), 5.48 and 5.66 (each non- The broad singlet peak of the enantiomer, 1H), 7.0 — 7.4 (m, 17H). &Lt; Please read the notes on the back first and then write this page) Printed by Beigong Consumer Cooperatives, Central Tabernacle Bureau, Ministry of Economic Affairs 1 3 C-N MR (δ 9 CD c 1 3) * &lt; 1 »(due to the two diastereomers> a pair of peaks were detected) 2 8» 2 f and 2 8 • 6 f 3 8 • 6 and 3 9 • 0 »4 5 ♦ 8 and 4 5 • 9 f 4 8 • 0 and 4 8 • 2 9 5 0 • 9 and 5 1 • 0 t 5 1 ♦ 4 and 5 1 • 5 t 5 5 • 2 and 5 5 • 8 9 6 0 • 3 and 6 1 • 1 and 6 1 • 2 t 1 2 6 ♦ 7 1 2 6 * 8 &gt; 1 2 6 • 9 ♦ 1 2 8 »6» 1 2 8 ♦ 8 t 1 2 8 • 9 »1 2 9 • 3 t 1 2 9 • 5 f 1 2 9 • 6 9 1 2 9 • 7 t 1 2 9 • 8 t 1 3 0 • 0 9 1 3 8 • 0 $ 1 3 8 • 2 t 1 4 5 • 0 t 1 4 5 • 2 t 1 6 7 • 3 and 1 6 7 «4 9 1 7 0 • 2 and 1 7 0 • 5 f 1 7 1 ♦ 0 and 1 7 1 • 0 5 • 1 7 3 • 0 and 1 7 3 • 1 0 IR (C m -1 f Κ Β Γ) • 1 7 2 3 p 1 6 6 7 and 1 6 3 5 (C = 0) 〇 The paper size is applicable to the 0 National Standard (CNS) A 4 specifications (210 X 297 mm) -175 A6 B6 Central Bureau of Standards, Ministry of Economic Affairs Printed by S Industrial Consumer Cooperative V. Description of Invention (173) MS (96): 640 (parent, 0.35), 452 (27), 3 7 6 (3 2), 2 6 4 (2 6), 1 9 3 (46), 120 (100), 91 (92). B. 1 one (N-the third butyl ethoxylamine) a 3-(2-amine even _3-Rongmou propionylamine) a 5. 7_ Errong a six-gas mixture 2-H equipment Add 950mg (1.49mni〇l) 1- (N- third butyl acetamide) -3- (2-(the third butane carbonyl amine group)-3-benzene to the 125mi bottom flask with N2 inlet Propylpropanamide) -5,7_diphenylhexahydroazazepine-2-one (a mixture of diastereomers) and 40 mi of ethyl acetate. The solution was cooled to Ot :, saturated with HCI gastris, and stirred at 〇〇 for 20 minutes, and then at room temperature for 40 minutes. The reaction was poured into aqueous sodium hydrogen phosphate solution, diluted with ethyl acetate, and the organic layer was washed with additional aqueous sodium hydrogen phosphate solution and brine, dried over magnesium sulfate and evaporated. Chromatographic separation of diastereoisomers on silica gel, using ethyl acetate / methanol as the eluent, produced oily diastereomers. The young diastereomers (R, = 0.4 in 10% methanol in ethyl acetate): a〇 = 28.2 ° (c = 1.5, CH 2C 1 2), 50% Yield. 2H — NMR (δ, CDC13): 1. 24 (single peak, 9H), 1 · 8 — 2. 6 (Limian multiple line, 4H), 3. 1 (m, 3H) »3. 58 (ABg, Jas = 16 »= 202, 2H), 3.59 (m, 1H), 4.18 and (please read the precautions on the back before writing this page) This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -176 α6 Β6 V. Description of the invention 4. 32 (multiple lines of two diastereomers, 1H), 5. 12 (d &gt; J = 1 0 t 1 Η) 9 5 • 1 7 (m $ 1 H) f 5 • 4 9 (b S »1 Η) f 7 • 0 — 7 • 4 (m» 1 5 H) 9 8 • 4 9 (d * J = 7 »1 H ) 〇1 3 Η -N Μ R (δ t CD c 1 3) • 4: 28.7, 3 9 • 2 »4 1 • 1 t 4 6 • 0 9 4 8 • 1 t 5 1 • 0 t 5 6 • 5 * 6 0 * 3 * 6 1 • 2 f 1 2 6 • 7 t 1 2 6 • 8 t 1 2 7 • 0 »1 2 8 • 4 9 1 2 8 • 6 t 1 2 8 • 9 t 1 2 9 • 0 t 1 2 9 • 3 t 1 2 9 • 5 t 1 3 7 • 8 t 1 3 8 • 1 $ 1 4 5 • 2 f 1 6 7 • 5 $ 1 7 3 • 5 ο IR ( C m -J »Κ Β Γ) • 1 6 6 5 and 1 6 3 5 (C = 0) 〇 Μ S (%) • 5 4 0 (Parent f 3) 9 4 4 9 (3 2) »3 7 6 (4 1) 9 2 6 4 (3 5) &gt; 1 9 3 (3 8) t 1 2 〇 (1 0 〇) f 9 1 (4 3) o Higher polar diastereomer (R f = 0 • 2 in 1 0 96 in ethyl acetate in methanol); α D 3 2 2 o (c = 1 • 5 (please read the precautions on the back before filling in this page) 丨 Binding-Order · Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs, CH2C12), 50% yield. 2H — NMR (δ, CDCla): 1. 23 (single peak, 9H), 1. 8 — 2 · 6 (continuous multiple lines, 4H), 3. 1 (m, 3H), 3.55 (m, lH) , 3.58 (AB ,, Jab = 16, Δ, = 220, 2H), 4. 18 and 4. 32 (multiple lines of two diastereomers, 1H), this paper scale is applicable to China National Standard (CNS ) A 4 specifications (210 X 297 mm) -177 21Π901 A6 B6 5. Description of the invention (175) 5 • 1 0 (df J zsz 1 0 f 1 H) 9 5 • 1 7 (m 9 1 Η) $ 5 ♦ 4 9 (b S 9 1 H) »7 • 0 1 7 • 4 (m 9 1 5 Η) 9 8 • 3 0 (dt J = 7 9 1 Η) 〇2 3 Η — NMR (δ» CDC 1 3) 4 4: 28.7, 3 9 ♦ 2 9 4 1 ♦ 2 9 4 6 • 0 9 4 8 • 1 1 5 1 • 0 t 5 6 ♦ 9, 6 0 »3 t 6 1 • 2 t 1 2 6 ♦ 7 $ 1 2 6 • 8 &gt; 1 2 7 • 0 »1 2 8 • 4 ί 1 2 8 • 6 9 1 2 8 • 9 f 1 2 9 • 0 9 1 2 9 • 3 t 1 2 9 • 5 9 1 3 8 • 1 f 1 3 8 • 2 t 1 4 5 • 1 $ 1 6 7 • 5 * 1 7 3 • 5 o IR (C m -i &gt; KB Γ) • ♦ 1 6 6 5 and 1 6 3 5 (C = 0) Ο Μ S (%) • 5 4 0 ( Parent 2) t 4 4 9 (3 7) 9 3 7 6 (5 3) t 2 6 4 (3 5) t 1 9 3 (3 5) 9 1 2 0 (1 0 0) t 9 1 (4 2) 0 C • (1 (N th T acetamide) 3 Amino mono 5 • 7 mono 5 phenyl hexaM xenon ketone (please read the precautions on the back and then f this page) 丨 Pack. Order · The central standard of the Ministry of Economic Affairs is an employee consumer cooperative printing a 100m round bottom flask equipped with a condenser and an N2 inlet. Add 0 · 40g (0 · 745 m following 〇1) 1-(N-third butylacetamide) A 3- (2-amino-3-phenylpropylamide) _5,7-diphenylhexahydroazazepine-2-one (higher polar isomer, from the above), 8 m 5 1 , 2-dichloroethane, and 0.093m5 (0.782mmol) phenylisomethane. Reaction reflux 1h r, cooling This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -178 A6 B6 21090. Fifth, the invention description (176), evaporation. The residue was ingested in 10m acetic acid and heated at 70-80t: 2hr. The reaction was cooled and the salt product was precipitated with ether and hexane. The precipitate was collected, dissolved in ethyl acetate, washed with aqueous sodium hydrogenate and brine, dried over sodium sulfate, and evaporated. Produced from chloroform solidified oil m p 204-2051C, 0.30g (10 0¾), cxd = -3.720 (c = 0.5, TFA) 〇 2H_NMR and; 3H — NMR spectrum is consistent with racemate. D. (+) — 1 one (N — third butyl acetamide) one makeup 5.7 7 — Errong a six-argon xenon xanthene leather 2- ketone as above, made from 1 one (N— third butyl Ethyl acetamide)-3- (2-amino- 3- phenylpropanolamine)-5, 7-diphenyl hexahydroazazepine-2- ketone (lower polar isomer) oil, Yield 92%, cxfl =

+ 3.21 ° (c = 0.8, ethyl acetate). iH — NMR spectrum is consistent with racemate. E. (one) one one one (N-the third buta Z · amide) one 3-(3-methionyl urea) one 5. 7-Errong six six-kid mixed leather one-2 In a 35mi round bottom flask with N2 inlet and condenser, add 293ng (0.745nmol) (—) — 1_ (N — third butylacetaldehyde amine) —3-amino-1,5-diphenylhexahydrogen Aza leather one 2-one, lOmi ethyl acetate, and 0. 096mi? (0. 745 mmoi) m-tolyl isocyanate. The reaction was refluxed for 2.5 hr *, cooled, and evaporated. The residue is chromatographed on silica gel using hexane / (please read note f on the back and then fill in this page> 丨 installation and ordering. Printed by the Ministry of Economic Affairs Central Counseling Bureau Employee Consumer Cooperative. This paper is suitable for troubled countries Standard (CNS) A4 specifications (210 X 297 g **) -179 Post 2 A6 B6 V. Description of the invention (177) Ethyl acetate is an eluent, producing oil, which is produced by the crystallization of methylene chloride / isopropyl ether m P 1 4 0 -1 5 0 υ, 7 1 (18¾) α Ό = 1 8 • 6 ° (C = 1, C Η 2C 1 2) 0 Τ R / value and lH--NM R on LC The spectra are proved to be racemates. Analysis and calculation of C 3 2 Η 38 Ν 4 0 3 · 1/2 Η 2〇: C 7 1 • 7 5, Η 7. 3 4, Ν 1 0 • 4 6 〇 Experiment • C 7 1 «6 6, Η 6 · 7 5 (-0 • 5 9), N 1 0 • 2 9 〇F • (+) 1-(Ν-flute = τ Hua acetamide)-3 (3 A (Zu urea)--5 · 7 Dizhu- ^ 1- »Gas argon M — ρ; ketone prepared as above from (+)-1 mono (N — butyl butylacetamide) mono 3 monoamine ― 5, 7 ― Diphenyl hydrazine leather 2 _ ketone oil $ 3 0% yield, which is produced by the crystallization of dichloromethane / isopropyl 9ί mp 1 4 0 ― 1 5 0 V, 15% yield »α ζ) = + 1 8 • 2 0 (c = 1 negative C Η 2C 1 2) Ο TLC R / value and 2 Η--Ν MR and 2 3Η NMR spectra are proved to be racemates. (Please read the precautions on the back and then write this page)-Pack · Order.

Analysis and calculation: CasHasNiOa · I / 2H2O: C 7 1. 7 5, Η 7. 3 4, N 10.46. Experiments: C 7 1. 6 5, Η 6. 8 9 (10. 4 5), Ν 1 0. 4 9 〇 Printed Example 7 1 (1-3 T Gas carbonylmethyl) 3-(3-Jiarong very urea and even the paper size is applicable to China National Standards (CNS) A 4 specifications (21〇X 297 mm) ΓΓΤ --- A6 B6 Central Bureau of Standards 8 Printed by the Industrial and Consumer Cooperatives V. Description of the invention (1 redundant)) 1 7 1 ring Γ3, Hua hydrogen argon mixed leather 1 2 —— n according to the example 1 1 white (1 ― third butane carbonylmethyl group) 1 3 monoamine Base 7 -cyclohexyl-ML · mm 雑 卓 一 2 ― Ketone 3 1% Yield »Μ • Ρ. 0 .8 a 1 • 0 (mt 2 Η) f 1 «1 a 1» 3 (m 9 4 H), 1 • 3 7 (S f 9 Η) f 1 • 6 a 1 • 9 (mf 1 0 Η ) 9 2 • 0 8 (m 9 1 Η) t 2 • 2 5 (s 9 3 H) 9 3. 4 2 (t, j = 7 9 1 Η) »3 • 8 8 (ABQ f J Λ B = 1 .7, Δ, 1 8 0 9 2 Η) f 5 • 0 1 (m 9 1 H), 6 • 6 5 and 7 • 1 7 • 4 (m 6 Η (broad single peak including 2 NH information)) ο 13 Η Ν Μ R (δ f CDC 1 3) * 4 21. 5, 2 5 * 7 &gt; 2 5 • 9 9 2 6 • 0 t 2 6 • 2, 2 7 • 2, 2 8 • 0 3 0 • 1 9 3 1 • 7 t 3 2 • 2, 3 9 • 4, 4 5 • 6, 5 1 «5 t 6 3 * 4 f 8 1 • 8, 1 2 3 .6 t 1 2 8 • 7, 1 3 8 • 7 9 1 3 9 • 1, 1 5 5 * 2, 1 6 8 • 4 Ο IR (C m -I f KB Γ) • 1 7 3 0 (c 0 2 R) and 1 6 4 0 (C 0 NR) o Μ S (96) • • 4 5 7 (2 t parent) f 2 9 5 (2 3 ) 9 1 8 5 (2 3) 9 1 0 7 (1 0 0) 0 H R M S Calculate c 2 6 H 4 0 Ν 3 Q 4 • 4 5 8. 2 9 8 4 〇 Experiment: 458.3057. (Please read the precautions on the back before filling in this page)-Packing · This paper scale is applicable to the national standard for troubled people (CNS> A 4 specifications (210 X 297 mm) -181 21 ^ 901 A6 _B6_ V. Description of the invention (179 ) Example 7 2 (1 a flute, tributyrin, a certain), a 3 — (3 — triturtomethyl, a certain), a urea), a 7 — a hexaargon gas mixed leather 2 —_ according to Example 11 prepared from (1-third butane carbonylmethyl)-3-amino-7-cyclohexyl hexahydroazazepine-2- ketone 36% yield, M. P. (please read the note on the back first ίItem and then fill out this page) 1 Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 1 1 4-1 1 7 1C 〇'H-NMR (δ, CDC13): 0. 8-1. Ο (m &gt; 2 H ), 1 • 1 one 1 • 3 (m • 4 H) 9 1 • 3 4 (S f 9 H), 1 • 6 — 1 • 9 (m »1 0 H) &gt; 2 • 0 (mt 1 H ), 3 • 4 8 (tt J = 7 t 1 H) »3 • 9 0 (ABQ 9 J Λ B =) -7, Δ, = 1 6 0 f 2 H)» 5 φ 0 4 (mt 1 H ) f 6 «8 — 8 • 0 (continuous multi-line» 6 H) Ο 1 3 H -NMR (δ 9 CDC 1 3): 25.7, 2 5 ♦ 8, 2 6 • 0 t 2 6 * 1 »2 7 1 f 2 7 • 9 Reference 3 〇 • 1, 3 1 • 5 6 t 3 1 • 6 3 f 3 9 • 5 t 4 5 • 7 »5 1 .3, 6 3 * 5 t 8 2 • 0 f 1 2 9 • 1 t 1 4 0 • 2, 1 5 4 * 8 f 1 6 8 ♦ 3 f 1 7 5 • 9 (non-specified all aromatic masters) o IR (C m -1 $ KB r) • • 1 7 3 0 (C 0 2 R) and 1 6 3 8 (c 〇NR) 〇MS (96) • 5 1 1 (&lt; 1 t parent) 9 2 9 5 (8 2) t 1 9 5 (2 8) 9 1 8 5 (9 8) f 1 6 1 (1 0 0) t 5 7 (9 7) o HRMS calculation C26H37N3〇4F3:. Installed. This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications ( 210 X 297 mm) -182 213901 A6 B6 Printed by the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (18〇) 512. 2732. Experiments: 512.2751〇 Fen_Example 7 3 (1 爮 三 丁 argon 或 certain a certain) a 3 — (3 — a certain rong urea) a fS. 7 — two argon six argon xenon heteroyl one 2 —_ Prepared according to Example 60 from (1-tert-butoxycarbonylmethyl) -3-amino-5,7-diphenylhexahydroazazepine-2-one, to obtain a foam of 6.3% yield. ^ -NMR (δ, CDC13): 1.2-1.4 (m, 2 Η), 1.2 9 (s, 9 Η), 2.0-2. 2 and 2.4-2. 6 (m, 2 Η), 2. 25 (s, 3 Η), 3. 21 (m, 1Η), 3. 60 (ΑΒ ,, J ^ = 18, Δ „= 1 6 0 (2 Η), 5. 1 5 (m, 1 Η), 5.22 (m, 1 Η), 6.8 and 7.0-7.4 (m, 1 6 Η) IR (cm-, ΚΒγ): 1723 (C〇2R) and 1 6 3 8 (C Ο Ν R) 0 MS (96): 527 (15, parent), 235 (30), 1 3 3 (1 0 0) 〇HRMS calculation C32H3rN3〇4: 527.2822. Experiment: 527.2742. Example 7 4 (1 焆 三 丁 argon carbonyl certain Shenmou) a 3 — (3 —A urea group (please read the precautions on the back before filling in this page) This paper scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 mm) -183 21:? ACl A6 B6 V. Description of the invention (181)) 5-stupid one 7-book base six hydrogen gas seal 2-Que A · 2-book base one 4 · A stupid spot P. sun according to Stork »G. and Dowd» SJ A ·. Che ·· Soc · »85, 2178 (1963) method. Equipped with N2 inlet, Dean-stark trap and condenser 250mi? Round 8.71g (50mrn〇l) 4-phenylcyclohexanone was added to the bottom flask, 5. 72πιβ (50 nmol) cyclohexylamine, and 100 mi? Benzene. The solution was refluxed until the water was completely removed (12 hours). The 20 mi? Cooled solution was added to the 1.0M ethyl magnesium bromide solution in Sigasan, Reaction at 60-70 t: heating for 30 minutes. Cooling the solution, adding 1.43m $ (12 mmol) sulfonyl bromide, resulting in an intermediate color change. The reaction was refluxed for 3.5 hours, cooled, and evaporated. The residue was taken up in 4 0 In mi IN HC 5, stir at room temperature for 18 hours, and extract in ethyl acetate. It is washed with water and brine, dried with sodium sulfate, and evaporated. The unprocessed yellow oil is no longer (please read the note on the back first $ Item then f this page) _Installation and ordering. Printed and purified by the employee consumer cooperative of the Central Standards Bureau of the Ministry of Economic Affairs and directly used t 3. 2 8 (1 0 0%) o 7 Η--NMR (d, CDC 1 3) • 1 • 6 2 (m 9 1 Η) t 1. 9 5 (m »1 H) • 2 • 2 0 (mt 2 H) f 2 • 4 1 (dd, J = 8. 5» 1 4 t 1 H) 9 2 • 5 5 (m, 2 H) 2. 7 7 (mf 1 H) 9 3 ♦ 0 1 (m, 1 H) • 3. 4 (dd »J = 4 t 14 9 1 Η) , 7. 0 -7 • 4 (mf 1 0 H) o IR (cm -1, KB r) • 1 7 1 5 (C = 0) 0 MS (%): 264 (parent, 38), 235 (10 The paper size is applicable to the Chinese National Standard (CNS> A 4 specifications (210 X 297 Mm) -184 213901 A6 B6 Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (182)), 1 5 9 (1 6), 1 4 6 (2 8), 1 4 5 (2 6 ), 131 (31), 1 0 4 (3 5), 9 1 (1 0 0) 〇B. 5—Rongmou 7—Shu Hexaargonium Complex Leather 2—one equipped with a condenser and N2 inlet In a 250-mi round-bottom flask, 2.64 g (10 mmol) 2-tertyl-4-phenylcyclohexanone, 1.70 g (15 off 〇1) hydroxylamine pair of sulfonic acid, and 50 mM formic acid were added. The reaction was refluxed for 5.5 hours, cooled and poured into 3N NaOH. The mixture was extracted into ethyl acetate, washed with brine, dried and evaporated. The residue was chromatographed on silica gel using formazan / dichloromethane to collect the product, R / = 0.30, oily, 1.8 g (64%). 2H-NMR (d, CDC13): 1.6-2.0 (m, 4H), 2. 57 (m, 1H), 2. 7 — 2. 9 (m, 4H), 3. 76 (m, 1H), 5 . 6 and 5. 75 ((broad single peak, NH_, 1H), 7.0 — 7.4 (m, 1 0 H) 〇IR (cm 'KBr): 1 6 6 0 (C = 0) 〇MS (% ): 279 (Parent, 13), 235 (24), 188 (4 0), 91 (1 0 0), 44 (3 1) 〇 The rest of the steps are the same as in Example 60: C · 3 — Gangyi 5 — Benji-7-Yeji Hexahydrogen Leather-2-1L oil, a mixture of 4 diastereoisomers, 27% yield. This paper scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 Mm) _ 1〇5 (please read 48 ^ surface note ^ | κ item and fill in this page) — Binding · Order-Γ A6 B6 2139G1 5. Description of the invention (183) i Η-NMR (δ, CDC 1 3): 1. 7-3.2 (connected multi-line, 5Η), 2.86 (m, 2Η), 3. 8 and 4.2 (multi-line, 1Η), 4.58 and 4.88 (Multiple lines, 1Η), 6.28, 6.55, 6.68 and 6.80 (broad single peak, NiL, 1Η), 7.0-7.4 (m, 10Η) o 23H — NMR (δ , CDC13): 4 diastereomers produce many overlapping peaks 170. 35, 170. 54 and 170. 65 appear 4 within 3 of the amide carbonyl group. IR (cm · , ΚΒγ): 1 6 7 0 (C = 0) MS (96): 358/360 (parent, Br79 / Β r 82 2/2), 266/268 (98X100), 2 2 2 (2 0) , 158 (4 5), 144 (53). D. 1— (The third butyl argon carbonylmethyl) —3-bromo—5-benzyl—7—sixyl six gas xenon complex leather—2-keto oil, 2/1 ratio of 2 diastereoisomer mixtures, 97% yield. 2H-NMR (d, CDCla): 1. 44 and 1. 45 (single peak, 9H), 1. 8 — 4. 3 (Continuous ore multi-line, 8H), 4.9 to 5.4 (multi-line, 1H), 7.0-7.4 (m, 1 0 Η) 〇IR (cm-i, KBr): 1745 and 1650 (C = 0). This paper scale is applicable to China National Standard (CNS) Grade 4 (210 X 297 mm) (please read the precautions on the back before filling out this page)-Pack. Order, Printed by the Staff Consumer Cooperative of the Central Bureau of Standards, Ministry of Economic Affairs -186 Ξ 2139GI α6 Β6 V. Description of invention # 84) MS (96): 392 (Parent-Br, 2), 372 (30), 2 5 5 (1 0 0), 2 0 0 (7 0), 180 ( 9 8). E. 1 one (the third butyl argon carbonyl methyl) one 3-arsenic 5-stupid one 7-fluorinated six gas mixture 2-keto oil, the ratio of 7/3 ratio of two kinds of diastereomers Isomer mixture, 87% yield. 2H-NMR (δ, CDC13): 1. 45 and 1. 46 (single peak, 9H), 1.8-4.6 (interlaced multiple lines, 9H), 7.0-7.4 (m, 10H). IRCcm- 'KBr *): 2 1 0 7 (N 3), 1739 and 1659 (C = 0) MS (96): 406 (Parent one N2, 2), 350 (10), 259 (13), 91 ( 17), 57 (16), 3 2 (1 0 0) 〇F. 1 a (third butyl argon carbonyl methyl) a 3- amine a certain 5-stupid a certain 7-Xieji six gas xenon mixed leather one 2 The oil is printed by an employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs, which is mainly a diastereomer with a yield of 67%. 2H-NMR (δ, CDC13): 1. 42 and 1.46 (single peak, 9H), 1. 5-2. 0 (m, 4H), 2. 32 and 2. 71 (multiple lines, 1H), 3. 08 (m, 2 Η), 3. 25 (m, 1 Η), 4.1 (m, 1 Η) -187 (please read the precautions on the back before filling in this page) -—install ·

• I This paper scale is applicable to the Chinese National Standard (CNS> A4 specifications (210 X 297 mm> 2139GI A6 B6. Printed by the Employees ’Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Invention Instructions (185)» 4 • 1 0 (ABJ B z =] L 7, Δ, = 75) t 7 • 0 — 7 • 4 (mt 1 0 H) 〇I 3 c — NMR (δ »CD Cl 3) 1 1» »(--diastereoisomer Structure) 2 8 • 1 »3 9 • 1 t 3 9. 3 t 4 4 • 7 t 5 1 • 8 9 5 4 • 3 f 5 5 • 4, 6 3 • 3 f 8 1 • 6, 1 2 6 • 7 »1 2 6 • 9 f 1 2 7 • 2 t 1 2 8 • 5» 1 2 8 «8 9 1 3 7 • 3 t 1 4 4 • 6 9 1 6 9 • 1 9 1 7 6 • 0 o Μ S (%) • 4 0 9 (Parent + 1 t 2) 9 3 6 2 (4 2) t 1 3 2 (1 0 0) 9 9 1 (3 0) 0 G 1 (Dibuti Carbonylmethyl) 3 (3 toluene hua P Hua) 5 benzene hua 7 benzhua 1-Hydrazine leather 2 m 9% yield t M • P. 1 0 0-1 1 0 t: o 2 Η--NMR (δ, CDC 1 3): 1 • 4 1 (st 9 Η) t 1 • 5-3 • 2 (continuous multi-line, 7 H) 9 4 * 1 5 (AB &lt; 1 t JAB =: 1 7, Δ v = 13 9) f 4 • 2 8 (mt 1 H) 9 5 • 2 4 (m $ 1 H) t 6 .8 and 7 • 0 -7 • 4 (m 9 1 6 Η) ο 13 C — NMR (δ 9 CD Cl 3) • * 2] L. 5, 2 8 • 0 9 3 8 • 2 t 3 9 • 3, 3 9 3 5 t 3 9 .4, 4 4. 5,5 0 .4, 5 5 • 6,8 1 • 9 9 12 7. 0, 1 2 7. 3. 1 2 8. 5, 1 2 8. 6,12 8. 7, 1 2 8. 9, 1 2 9. 0, 1 3 6. 7, (know the precautions on the back and then fill out this page). Pack. Order · • — \ Λ. This paper size is applicable Nursery National Standard (CNS) Grade A 4 (210 X 297 mm) -188 V. Description of invention (186) A6 B6 Printed by the Employees Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 1 3 8 • 9 »1 4 4 • 4 9 1 5 5 • 3 »1 6 8 • 6» 1 7 3 Ο IR (cm -2 »KB r) • 1 7 4 0 (C 0 2 R) and 1 6 4 0 (c ONR) 0 Μ S (%) • 5 4 1 (parent t 2) 9 2 6 1 (3 0) 9 1 3 2 (1 0 0) t 9 1 (4 7) 〇Analysis calculation c 3 3 H 3 9 N 3 (D 4 • C 7 3 • 1 7 9 H 7 • 2 6 $ N 7 • 7 6 〇Experiment • • C 7 2 ♦ 8 2 t H 7 • 2 8 f N 7 • 7 1 〇 賨 Example 丨 7 5 (1-the third butane gas carbamide ) — * 3 __ (3 methamphetamine) 5 Benhua 7 Hua—L. Argon xenon leather 2 m White compound prepared according to the method of Example 6 0 17 4 F 9 9 7 7 Yield 9 Μ Shu P ♦ 9 5 1 1 0 5 V 〇i Η--NMR (δ, CS DC] 3): 1 • 4 0 (sf 9 Η) 1 • 5 — 3 • 2 (tandem multi-line t 7 Η ) 9 3 • 7 2 (S f 3 H) 9 4 • 1 0 (A Β Q 9 J Λ B = =) [7 9 △ V = 1 3 5) $ 4 • 2 8 (m 9 1 Η) f 5 • 2 4 (m »1 Η) 9 6 • 5 &gt; 6 • 8 and 7 • 0 — 7 • 6 (m 9 1 6 Η) 0 13 C-N Μ R (δ 1 CDC 1 3): 28 . 0, 3 8 • 2 9 3 9 «2 f 3 9« 3 9 3 9 • 4 9 4 4 ♦ 5, 5 0 4 9 5 5 * 2 see 5 5 • 7 t 8 2 0 1 0 5 .4 The size of this paper is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 mm) (please read the notes on the back first Matters will be written on this page) -189 21: i9C〇A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of Invention (187) t 1 0 9 • 2 9 1 1 2 * 2, 1 2 6 ♦ 9 t 1 2 7 • o, 1 2 7 • 2 »1 2 7 • 3, 1 2 8 • 5» 1 2 8 • 6 »1 2 8 • 7 f 1 2 8 • 9, 1 2 9 • 1» 1 2 9 • 2 t 1 2 9 • 3 9 1 2 9 • 5, 1 2 9 • 6 9 1 3 6 • 7 t 1 4 0 • 4 y 1 4 4 «4, 1 5 5 • 2 t 1 6 0 • 2 t 1 6 8 ♦ 6 t 1 7 2 ♦ 9 0 IR (cm -i $ KB r) «• 1 7 4 0 (C 0 2 R) and 1 6 4 0 (c 0 NR) ο Μ S ( %) • • 5 5 7 (parents • 1) »2 6 1 (3 5) f 1 4 9 (1 0 0)» 1 3 2 (9 8) »1 2 3 (5 3) f 9 1 ( 5 2) o Analysis calculation c 3 3 H 3 9 N 3 0 5 C 7 1 • 0 7 f Η 7 • 0 5 f N 7 • 5 3 〇 Experiment • C 7 1 • 3 0 9 H 7 • 1 0 t N 7 • 3 4 0 Night Example 7 e (1 _ third T argon carbonyl ^) 3 (3 monophenyl urea ^) 5 Phenol 7 Hua _IU Radon cyanide leather 2 ketone The white compound 7 4 F of Sassafras was prepared according to the method of Example 6 0 9 3 3% yield t Μ • P • 9 5 — 1 10 〇1 Η--NMR («5, CDC] 1 3) • 1 • 3 8 (s I 9 Η) f 1 • 5 — 3 • 2 (connected multi-line »7 Η) 9 4 • 1 0 (ABQ 9 J. B = 1 7, △, 13 8) f 4.38 (m, lH ), 5.28 (m, lH), 6.8 (please read the precautions on the back before filling in this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -190 B6 Central Standard of the Ministry of Economic Affairs Printed by the Bureau ’s Consumer Cooperatives V. Description of inventions (188) — 7 • 8 (m 9 1 6 Η) Ο 13 C — NMR (δ 9 CDC 1 3) • • 2 8. 0, 3 7 • 5 9 3 9 • 1 t 3 9 • 2, 3 9 • 5 $ 5 0 • 3, 5 5 • 7 9 6 0 • 4 f 8 2 • 1 f 1 1 7 • 3 9 1 1 9 • 4 9 1 2 2 • 3 9 1 2 2 • 4 t 1 2 6 • 5 t 1 2 6 • 7 9 1 2 7 • 0 9 1 2 7 • 1 1 2 7 • 2 t 1 2 8 • 5 9 1 2 8 • 6 t 1 2 8 • 8, 1 2 8 • 9 f 1 2 9 • 2 f 1 2 9 • 3 ί 1 2 9 • 7 f 1 3 4 • 4 9 1 3 6 • 6 9 1 4 0 • 6 9 1 4 4 • 2 t 1 5 5 • 0 »1 6 8 • 5 f 1 7 3 • 6 0 IR (cm -1 f κ Β Γ) • • 1 7 4 0 (c 0 2 R) and 1 6 4 0 (c 0 NR) ο Μ S {%) • 5 6 2 (parent 9 1), 2 6 1 (5 0) ref 1 5 3 (8 0) 9 1 3 2 (1 0 0), 9 1 (4 0) o Η R Μ S calculation c 3 2 Η 3 7 Ν 3 0 4 C 1 • • 5 6 2 • 2 4 7 6 5 ο Experiment 5 6 2 • 2 4 9 7 0 Ο Analysis calculation C 3 2 H 3 6 Ν 3 0 4 C 1 • • c 6 8 • 3 8, H 6 • 4 6 f N 7 • 4 8 0 experiment • C 6 8 • 3 7 H 6 • 7 6 t N 7 • 0 2 (— 0 • 4 6) o ΜΜ 7 7 (1 mmmm zr T m carbonylmethyl) 3 one (3 toluene hua m hua) 5 MM 7 瑗 has a certain methyl hexamethane m heterolog 2 ketones according to examples The 74 method is prepared from (1-3rd butane carbonylmethyl)-3-(please read the note on the back first and then write this page) The paper size and degree are applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -191 A6 B6 V. Description of the invention (189) Aminyl 5-phenyl-7-cyclohexylmethyl Leather hexahydroazepino a 2-keto-foam yield of 47%, diastereomeric mixture. Printed by the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 1 Η--NMR (δ, CDC 1 3) • 1 • 3 7 (s »9 Η) t 0 • 8 1 2 • 3 and 2 • 6 4 Line> 7 H) 9 3 • 1 8 (m »1 H) f 3 • 9 5 and 4 • 0 (A Β • &lt; 5Ε s» JAB = 1 7 and 1 7 &gt; △ V = 1 3 9 And 1 5 0) »4 ♦ ○ 4 • 1 (m 9 1 H) t 5 t 1 2 and 5 • 2 3 (multiple \ heavy line> 1 H) t 6 • 8 and 7 • 0 — 7 • 5 (mt 1 6 H) 〇i 3 c-NMR (δ fc DC 1 3) «• (--diastereomer) 2 1 • 5 t 2 6 • 1 9 2 8 • 0» 3 3 • 3 »3 3 • 5 f 3 4 • 6 3 9 • 2 t 3 9 • 3 t 3 9 • 9 t 4 1 • 5 t 4 4 • 9» 4 6 • 0 9 5 1 • 9 t 5 4 • 2 9 8 1 • 8 »1 1 7 • 1 9 1 2 0 • 8, 1 2 3 • 6 9 1 2 3 • 8 t 1 2 6 • 3 t 1 2 6 • 4 f 1 2 6 • 9 f 1 2 7 • 2 9 1 2 8 • 5 f 1 2 8 «7 9 1 3 8 • 7 t 1 3 9 • 1 9 1 4 4 • 8 9 1 4 5 • 6 f 1 5 5» 1 f 1 6 8 • 5 f 1 7 3 • 3 〇IR (cm -1 »KB r) • 1 7 4 0 (C 0 2R) and 1 6 4 0 (c 0 NR) 〇 M S (96): 5 4 7 (parent t 1) 9 2 4 3 (1 5) 9 1 8 4 (5 0) 9 1 4 1 (3 0) »1 3 6 (1 0 0) Ο Analysis and calculation C33H45N3〇4: C 72. 36, Η (Please read the precautions on the back before filling this page) This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -192 21390- 'Α6 Β6 V. Description of the invention (190) 8. 2 8, N 7. 67. Experiment: C 72. 21, Η 8.35, Ν 7.44. Fenshi Example 7 8 (1 a third butyl argon carbonyl methyl) a 3 — (3-methyl carbazide urea) a 5 —juki a 7 —cyclohexyl hexaargon 氤 璤 箪 -2 —one according to Example 74 Method Prepared from (1-third butane carbonylmethyl-3-amino-5-phenyl-7-cyclohexyl hexahydroazazepine-2-ketone 6% yield 3/1 diastereomer Mixture, foam. (Please read the precautions on the back before filling this page) Printed by the Ministry of Economic Affairs Central Standards Bureau Beigong Consumer Cooperative 2 Η--NMR (δ, CDC 1 3) • 0 • 8 —— 2 • 3 ( m 9 1 5 H) f 1 • 3 7 (S »9 H) f 2 • 2 6 (s, 3 Η) 3 • 0 2 and 3 • 2 2 (multi-line f 1 H) t 3 .6 (mt 1 H) f 4 • 0 1 and 4 • 1 (AB 9 »JX b = 1 7 and 1 7 t △ V = 2 1 6 and 2 3 0 2 H)» 4 • 9 2 and 5 • 1 3 (multiple Line $ 1 H) f 6 ♦ 7 a 7 • 4 (m ， 1 H) ο J 3 C — NMR (df CDC 1 3) &lt; 1 &gt; »(--diastereomer) 2 1 • 5 9 2 5 • 8 6 »2 5 • 9 0 2 6 • 1 9 2 8 • 0» 3 1 • 5 9 3 9 • 4 9 3 9 • 9 9 4 5 • 8, 4 6 • 6 &gt; 5 1 • 6 * 6 3 • 1 »8 1 • 9 t 1 1 7 .2 * 1 2 0 • 8 t 1 2 0 ♦ 9 &gt; 1 2 3 • 6 t 1 2 3 • 8, 1 2 6 • 4 9 1 2 6 • 9 t 1 2 7 • 0 $ 1 2 8 • 5 t 1 2 8 • 6 t 1 2 8 • 7 t 1 2 8 • 8 9 1 3 8 • 8 t 1 3 9 • 0 f 1 4 5 9 9 1 5 5 • 1 9 1 6 8 2 t This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -193 A6 B6 21 ^ 03. V. Description of the invention (191) 17 5 . 5 〇IR (cm ·, KBr): 1730 (C〇2R) and 1 6 4 0 (CONR) 0 MS (%): 533 (parent, 2), 240 (25), 1 3 3 (1 0 0), 107 (70), 91 (40) 〇HRMS calculated C32H43N304: 533.3243. Experiment: 533. 32941. Example 7 9 (1-third T 鰊 馊 甲某)-3-(3-methyl qirong urea)-5-Zhu mou 7-瑗 hexyl six gas mixed leather-2 according to Example 74 Prepared from (1-tertiary butane carbonylmethyl) -3-amino-5-phenyl-7-cyclohexylhexahydroaza-2-2-one 14% yield, diastereomeric mixture, foam. 2H-NMR (δ, CDC13): 0. 8-2. 3 ((Please read the precautions on the back before writing this page) — Pack. Order_ Printed by the Ministry of Economic Affairs Central Standards Bureau Employee Consumer Cooperative M 9 1 5 Η) y 1 • 3 7 (S t 9 H) »2 .6 (mt 1 Η) &gt; 3 • 0 ― 3 • 4 (mt 1 H) 9 3 .7 4 (s, 3 Η)» 3 • 9 7 and 4 • 1 (AB 9 s 9 JAB = 1 7 and 1 7 &gt; Δ υ = 2 1 3 and 2 4 0 9 2 H) 9 4 .9 0 and 5 • 1 2 (multiline »1 Η ) 9 6 • 5 and 6 • 8 ― 7 • 4 mf 1 1 Η) 1 3 c-N MR (δ t CDC 1 3) • • (--diastereomer) 2 5 9 t 2 6 * 3 f 2 8 0 f 3 1 .0 * 34. 9, 42. 5, 45. 8, 46. 6, 51. 5, This paper scale is applicable to China® Home Standard (CNS> A 4 specifications (210 X 297 Gong * &gt; -194 A6 B6 Printed by the Employees Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs

V. Description of the invention (192) 55.2, 63. 1, 64.7, 81.8, 1 0 9.0, 1 2 6. 2, 1 2 6. 3, 1 2 6. 9, 1 2 7. 0, 128.5, 128.6, 1 2 9. 5, 129.6, 1 4 0. 5, 1 4 5. 9, 1 4 7. 1, 1 5 4. 9, 160.2, 168.3, 175.4. IR (cm-1, KBr): 1730 (C〇2R) and 1 6 4 0 (C Ο NR) 〇MS (%): 549 (parent, 3.5), 344 (25), 2 4 0 ( 3 0), 149 (6 0), 132 (10 0). HRMS calculation C32H43N304: 549.3 1 92. Experiment: 549.33256. Fen Shi Example 8 0 Shunyi 1— (third butyl ethyl amine) —3-(3-tolyl gland even) —5_Mothyl 7— (4 argon Rongmou) Hexaargon 氤 皮 1-2 — _ Prepared according to the method of Example 60 from cis-1-1- (third butylacetamide) -3 monoamino-5—phenyl-7— (4-fluorofluorophenyl) hexahydroazazepine-2 1-one 63 % Yield, M.P. 228-232¾. iH-NMR (δ, CD3SOCD3): 1. 16 (single peak, 9H), 2. 0 (s, 3H), 2. 24 (s, 3H), 2. 5 (m, 1H), 3. 1- 3. 9 (multiple lines, 3 H), 5. 10 (m, 1 H), 5. 34 (m, 1 H (please read the precautions on the back before writing this page)-丨 Install · Order-This The paper scale is applicable to the Chinese National Standard (CNS> A4 specification (210 X 297 mm) -195 Central Bureau of Standards®: Printed by the Industrial and Consumer Cooperatives V. Description of Invention (193)), 6. 6-7. 5 ( m, 1 4 Η), 8. 95 (bs, 1 Η) 〇i3C-NMR (δ, CD3SOCD3): 21. 3, 28.4, 45.0, 50. 0, 5 1. 6, 5 8. 5, 114.7, 115.1, 115.4, 118.1, 121.8, 122.4, 126.3, 126.8, 128.5, 131.6, 131.7, 135.5, 137.8, 1 4 0.5, 146.2, 154.1, 167.2, 173.4. IR (cm ^, KBr): 1660 (width, C = 0) Ο FAB MS (%): 545 (parent +1, 43), 4 7 2 (3 6), 4 1 2 (3 7), 2 5 4 (2 7), 2 11 (10 0) 〇 Analysis and calculation of C32H37N4〇3F · 3 / 4Η2〇: C 68. 86, Η 6.95, N 10. 04. Experiment: C 68. 87, Η 6. 8 6, Ν 9 · 69〇 Example 8 1 Shun Yi 1 Yi (絮 三 丁某 acetamide)-3-(3-methyl argonine base)-5 -Phenyl-7- (4-monophenyl) six-gas mixture leather 2-one ketone was prepared from cis-1-1- (third butylacetamide) -3-amino-5-phenyl 7_ (4_ 氤 phenyl) Hexahydroazepine leather 1 (Please read the notes on the back first and then write this page) The paper size is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -196 A6 B6 V. Description of the invention (194)-54% yield of ketone, Μ · Ρ · 224-227Ό. 'H-NMR (δ, CD3SOCD3): 1. 16 (Central Bureau of Standards of the Ministry of Economic Affairs®: Printed by the Industrial and Consumer Cooperative

Single peak 9 9 H) 9 2 • 0 (m &gt; 3 H) 9 2 • 6 (m 9 1 H) »3 • 2 — 3 • 9 (m» 3 H) t 3 • 7 0 (sf 3 H ) 9 5 • 1 0 (m »1 H) 9 5 ♦ 3 2 (mf 1 H) t 6 • 5 and 6 • 8 — 7 • 5 (m» 1 4 H) 9 9 • 0 5 (b S 9 1 H) 〇13 c — NMR (δ 9 CD 3 SOCD 3) • • 2 8 # 4 t 4 4 • 9 9 4 6 • 8 »5 0 • 0» 5 1 • 5 9 5 4 • 9 t 5 8 • 5 9 1 0 3 • 2 »1 0 6 • 5 t 1 0 9 • 9 t 1 1 5 • 1 &gt; 1 1 5 • 4 t 1 2 6 • 3 1 2 6 • 8 9 1 2 8 • 5 f 1 2 9 • 4 t 1 3 1 • 6 t 1 4 1 • 8 t 1 4 6 • 1 f 1 5 4 • 1 t 1 5 9 • 7 9 1 6 7 • 2 9 1 7 3 »3 o IR (C m -1 9 KB Γ) • 1 6 6 0 (寛 f C = 0) 〇FABMS (%): 5 6 1 (parent + 1 t 2 5) 9 4 8 8 (3 0) f 4 1 2 (2 8) f 2 5 4 (2 7) »2 1 1 (1 0 0) o Analytical calculation C 3 2 H 3 7 N 4 0 4 • H 2 0: C 6 6. 4 2» Η 6 • 7 9 t N 9 ♦ 6 8 O experiment * »C 6 6 • 3 6 9 Η 6 • 5 7 9 N 9 • 4 2 O (Please read the precautions on the back before filling in this page) Example 8 of Fen Shi 2 This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) _ 1〇7 21 ^ 90 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of inventions Shunyi 1 1 (3rd Dinghua B mm) 1 3 (3 Qi Binghua m) 5 Dinghua 7 (4 gas benzene water chestnuts) Oxyazazepine extraction-ϋ_ according to Example 6 0 method to prepare Baishun-1 1 (third butylacetamide) — 3 — amino-1 5 monophenyl — 7 1 (4 monophenyl) m aza leather-2 — Ketone 4 4% yield * M • Ρ • 1 7 5 — 1 7 8 V 〇2 Η--NMR (δ, CD 3 S 0 CD 3) «1 • 16 (early peak t 9 H) * 2 • 0 (m »3 Η) y 2 • 6 (m, 1 H) 9 3 • 2-3 • 9 (m» 3 Η) t 5 • 1 0 (m, 1 H) 9 5 • 3 2 (m 9 1 H) $ 6 ♦ 8-7 • 6 (m, 1 4 Η), 9 • 2 7 (bst 1 Η) 〇1 3 C-N MR (δ 9 c DC 1 3): 28.4 5 4 4 • 9 »4 6 • 8 &gt; 5 0 0 9 5 1 • 6 t 5 8. 5 t 1 1 5 ♦ 1 »1 1 5» 4 f 1 1 5 • 8 &gt; 1 1 6 .8 »1 2 〇 • 7 9 1 2 6 • 4 t 1 2 6 * 8 t 1 2 8 .6 t 1 3 0 • 3 t 1 3 1 • 6 9 1 3 1 • 7 t 1 3 3 .2 t 1 3 5 • 4 $ 1 4 2 • 1 1 1 4 6 • 1 9 1 5 3 .9 »1 6 7 • 2 t 1 7 3 • 2 0 IR (cm -1» κ B Γ) • • 1 6 6 0 (wide parameter C = 0) 〇FAB Μ s (96 ) • 5 6 5 (parent t 2 0), 4 9 2 (2 6) »4 1 2 (2 7)» 2 5 4 (2 0) »2 1 1 (1 0 0) 〇Analysis calculation C 3 1 H 3 4 N 4 0 3 FC 1 ♦ 2 Η 2 0 ： c Note The paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -198

I page binding Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 2.13 9 Ο ^ α6 _Β6_ V. Description of the invention (196) 61.94, Η6.37, Ν9.32. Experiment: C 6 1. 9 3, Η 5. 73 (-0. 64), Ν 9. 0 9 〇 HRMS calculation C3iH34N4〇3FC 1: 564.2790. Experiment: 564. 23444. Fenshi Example 8 3 shunyi 1-1 (the third butyl acetamide) a 3- (3-methyl ureido) a 5 ~ ~ phenyl a 7-(4-gas phenyl) six-gas mixed leather ~~ 2-Ketone is prepared from cis-1-11 (third butylacetamide) -3 monoamino-5—phenyl-7— (4-aminophenyl) hexahydroazatrile-2 according to Example 60 One ketone 69% yield, M.P. 224-226TC. ^ H-NMR (δ, CDC13, TFA): 1. 20 (please read the precautions on the back before filling in this page) (Zaofeng> 9 Η) 2 .0 (m, 1 H) 9 2. 3 ( m, 3 Η) t 2 .3 3 (s, 3 H), 3. 3 0 (m, 1 H) 9 3 • 9 8 (AB &lt; it J Λ s = 1 6, Δ „= 43, 2 H) t 5 • 2 7 (m 9 1 H) t 5. 3 8 (d, J = 1 1, 1 Η) 9 6 .6 9 (d, J = 7, 1 H), 6. 9 —

7.5 (m, 1 6 Η) ○ &quot; C-NMR (δ, CDC13, TFA): 22. 0, 27. 9, 38. 5, 38. 8, 45. 6, 52.8, 61.0, 112.4, 116.1, 119.9, 126.6, 127.3, 128.9, this paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) _ 1 QQ A6 B6 Central Standards of the Ministry of Economic Affairs W Wong Consumer Cooperatives Printing Department V. Description of Invention (197) 1 2 9. 5, 129.8, 130.8, 1 3 4. 9, 143.6, 1 5 8, 1 7 6 〇IR (cm ·, KBr): 1660 (width, C = 〇) 〇FAB MS (% ): 561 (parent +1, 47), 4 8 8 (3 0), 4 5 4 (2 0), 4 2 8 (2 5), 2 2 7 (2 8), 1 5 7 (1 0 0), 119 (4 6) 〇 Analysis and calculation of C32H37N4〇3C 1 ♦ 1 / 2Η2〇: c 67.41, Η 7.2, Ν 9.83. Experiment: C 67.77, Η 6.57, Ν 9.44. Endeavour Example 8 4 lf-1 1 (disanbutyric acid tyramine) 1 3-(3-methyl benzene stupid · Mian mou) 5-cage group 7-(4-phenyl) six gas Miscellaneous leather one lion according to the method of Example 60 prepared from cis-1 1 (third butyl acetamide)-3 monoamino 5-phenyl 7-(4-gas phenyl) hexahydroaza leather 2 • 33% yield of ketone, M.P. 130-132Ό. 'H-NMR (δ, C Ό C \ 3t TFA): 1.21 (single peak, 9H), 2. 0 — 2.4 (multiple lines, 4H), 3. 29 (m, 1 Η), 3. 82 (s , 3 Η), 3. 89 (ΑΒ ,, J λ Β = I 6, Δ, = 77, 2Η), 5. 24 (m, 1 Η), 5.39 (d, J = 1 1, 1 Η ), 6 · 7 — 6. 9 and 7. 1— 7. 4 (m ， 16Η) 0 (please pay attention to the precautions first, and then go to this page>. Packing. The size of the revised paper applies to the Chinese National Standard (CNS ) A4 specifications (210 X 297 g ** one 200 A6 B6

V. Description of the invention (198) 1 3 C — Ν MR (δ CDC 1 3, TF 'A) * • &gt; &gt; 2 8 • 0 t 3 8 • 7 9 3 8 • 9 t 4 5. 6 f 4 8 • 3 f 5 2 • 6 9 5 2 • 8 9 5 5 • 5 »6 0. 8» 1 2 6 • 6 t 1 2 7 • 3 t 1 2 8 «9 1 1 2 9 .5 f 1 3 0 • 4 9 1 3 0 • 5 9 1 3 0 • 8 $ 1 3 5 • 1, 1 3 5 • 6 * 1 4 3 • 8 t 1 6 0 • 2 f 1 6 8 • 8, 1 7 5 • 7 〇IR (cm -1 9 KB r) • 1 6 6 0 (width t C = 0) 0 FABM s (%) • 5 7 7 (parent f 8 2) 9 (please read the precautions on the back first (Fill in this page) Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 5 0 4 (6 1), 4 2 8 (5 6), 2 2 7 (7 6), 119 (10 0), 103 (5 5) 〇 Analysis and calculation of C 37N 4〇4C 1: C 6 6.6 0, Η 6. 4 6, Ν 9.71. Experiment: C 66.83, Η 6.46, Ν 9.51. Fen Shi Example 8 5 cis-1 1 (tributyltriethylacetamide)-3-(3-atmosphere jasmyl ureido)-5-phenyl 7-(4- atmosphere phenyl) six-gas mixed leather- 2 — ®L Yield according to Example 60, M.P. 229_231t :. ^ -NMR (δ, CDC13, TFA): 1. 21 (single peak, 9H), 2.0-2.4 (multiple lines, 4H), 3.2 9 (m, 1Η), 3.92 (ΑΒ ,, J αβ = 1 6, Δ, = 65, 2 Η), 5. 27 (d, J = 8, 1 Η)-Binding _ Order-This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -201 A6 B6 5. Description of the invention (199) 5 • 4 3 (d 9 J = 1 0 9 1 H) 9 7 • 1 1 7 • 5 (mt 1 6 H) o 1 3 C — NMR (δ &gt; CDC 1 3, TFA) • 2 2 • 0 9 2 7 • 9 9 3 8 φ 7 »4 5 • 6» 4 8 • 3 t 5 2 • 5 9 6 0 • 9 »7 1 • 3 $ 1 2 6 • 1 &gt; 1 2 6 • 6 &gt; 1 2 7 • 3 t 1 2 8 • 9 »1 2 9 • 5 t 1 3 0 • 6 t 1 3 〇 • 8 f 1 3 4 • 9 1 3 5 • 3 9 1 3 5 • 7 »1 4 3 • 7 t 1 7 6 • 0 OIR (cm -1 * KB Γ) 1 6 6 0 (width 9 C = 0) 〇FABM s (96) : 5 8 1 (parent + 1 »6 3) t 5 0 8 (6 1)» 4 2 8 (3 6) 9 2 2 7 (6 5) t 1 2 7 (8 1) 1 1 9 (1 0 0) O Analysis calculation c 3 1 H 3 4 N 4 0 3 C 1 2 '1 / / 3 H 2 Ο • c 6 3 • 3 7 9 H 5 * 9 5 N 9 • 5 4 〇 experiment • • c 6 3 • 7 4 H 5 • 9 9 9 N 8 • 8 7 (one 0 • 6 7) Ο Η RM s calculation c 3 1 H 3 4 N 4 0 3 C 1 2: 5 8 0 • 2 0 0 8 0 experiment ♦ • 5 8 0 1 9 9 4 0 Ο (please read the precautions on the back before filling this page) Ministry of Economic Affairs Printed by the Central Bureau of Standards, S Industry and Consumer Cooperatives Example 8 6 Shunyi 1 1 (the third butyl ethylacetamide) 3— (3 —toluene yimou) 5 —Mo 7 7 — (4 1 Jia Mo Certain) Hexaargon Xenon Zinc One 2 —

IL This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm> -202% Α6 Β6 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Description of Invention &lt; 2〇〇) According to Example 6 0 Method for preparing Baishun— 1 mono (third butylacetamide) — 3 —amino group — 5 — phenyl group 7 — (4 — tolyl group) *-Hydrazine leather 2 2 one ketone 5 7% yield t M • P • 2 1 6-2 1 8 V 〇1 Η--NMR (δ, CDC] 3 &gt; TFA) • 1 • 2 0 (9 9 Η) »2 • 0 — 2 • 4 (multiline 9 4 Η) 1 2 • 3 3 (s 9 3 H) &gt; 2 • 3 4 (S »3 Η) 9 3 • 2 7 (mt 1 H)» 3 ♦ 9 6 (AB 4 9 r Λ Β = = 1 .6 9 Δ V = 6 2 f 2 H) 1 5 • 2 2 (d »J = 1 0» 1 Η) »5 • 3 9 (d 9 J = 1 0 $ 1 Η) t 7 • 0 1 7 • 4 (m »1 6 Η) 〇1 3 C — NMR (δ» CDC 1 3 t TFA) 2 0 • 9 t 2 2 • 0 f 2 7 • 9 f 3 8 • 5 »3 8 • 9 f 4 5 «7 9 4 8 • 2 t 5 2 • 8 t 6 1 • 5 t 7 1 ♦ 3 * 1 2 0 • 8 &gt; 1 2 4 • 5 1 1 2 6 • 6 1 1 2 7 • 2 t 1 2 8 • 0 t 1 2 8 »9 t 1 2 9 • 3 1 1 2 9 ♦ 8 9 1 3 0 • 0 9 1 3 3« 4 , 1 3 4 • 7 1 3 9 • 7 f 1 4 0 * 4 f 1 4 3 • 9 t 1 7 6 0 IR (cm -1 9 KB r) • • 1 6 6 〇 (width f C = 0) 〇FABM s (%): 5 4 1 (parent + 1 $ 1 0) t 2 0 7 (1 2) t 1 5 7 (1 0 0) 1 1 9 (2 4) f 1 0 3 (1 2 ) o Analysis and calculation of C 3 3 H 4 0 N 4 0 3 • C 7 3 • 3 0 »Η 7.46, N 10.36. Experiment: C 72.90, Η &lt; first read the note on the back and then write this page) This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -203 A6 B6 _ V. Invention Explanation (201) 7. 3 7, N 10. 1 1 〇 Fen case 8 7 cis-1 1 (third butylacetamide)-3-(3-Shen g Zhumou gland)-5-phenyl A 7 -_ (4 a tolyl) hexaargon gas hetero-K-ρ; ~ ini According to the method of Example 60 prepared from cis-1 1 (third butylacetamide)-3 monoamine 5-phenyl 7 — (4-tolyl) Hexahydroazepine-2-4 0% yield of amorphous solid. ^ -NMR (δ, CDC13, TFA): 1. \ g (single peak, 9H), 2. 0-2.4 (multiple lines, 4H), 2. 3 4 (s, 3 H). 3. 29 (m , 1 H), 3. 83 (s, 3H), 3.95 (AB ,, J “= l6» Δι, = 81 »2H)» 5. 22 (d * J— 11, l ^ j), 5.40 (d, J = 1 1, 1 H), 6. 8 and 7. χ ~ * 7.4 (m, 16H) 〇i3C-NMR (δ, C Ό C \ a, TFA): (please read the back Please note that this page will be written again. -Installed. Ordered — — Printed by the Central Bureau of Standards, Ministry of Economic Affairs, 8 Industrial and Consumer Cooperatives 8 12 5 9 3 6 ♦ ♦ ·, 703 6 5 2 3 4.. 111 00, 〇3 5 6 0 7 8, ···· 9 7 6 0 9 5. · 2 3 3 7 7— ix 1- 1 ± 1X 2 5 »*» »,, 2 344 0 2 ···· . 6 9 3 9 2 8 2 2 3 6 241 1 1 1 p fee 6 2. 9 6 2 51 ♦ 4 7 8 0 7, »2 3 5 9 4 111 &gt; &gt;

m c R I

Γ B K

o II c wide / l \ o 6 6 1X sheets of paper, printed by a quasi-oak family, country, country and middle school, printed by the Ministry of Economic Affairs t Central Standards Bureau employee consumer cooperative. a6 _B6_ V. Invention description (202) 0 FAB MS (%) : 557 (parent +1, 59), 4 8 4 (4 5), 4 0 8 (4 3), 2 5 0 (3 2), 2 0 7 (1 0 0), 132 (3 3), 1 0 5 (4 3) 〇 Analysis and calculation of C 33H wN 4〇4 ♦ H 2〇: C 68.97, H 7. 3 7, N 9. 75. Experiment: C 68.97, Η 7.38, Ν 9.60. Fen Shi Example 8 8 Shunyi 1— (third butyl acetamide) —3— (3—3—benzene, urea) —5—Rongji—7— (4—1 rong) Hexaargon xenon Leather 2-Ketone is prepared from cis-1 1 (third butylacetamide)-3 monoamine 5-phenyl 7-(4-tolyl) hexahydroazepine leather 2 1 according to the method of Example 60 Amorphous solid with 41% yield of ketone. 'H-NMR (δ, C Ό C \ 3, TFA): 1.20 (please read the precautions on the back before filling in this page). Pack. Order. 丨 ((αο 早 峰 f 9 Η) &gt; 2 • 0 One 2 • 4 (multiple line, 4 H), 2 • 3 4 (s 9 3 H) 9 3 • 2 9 (m, 1 H) 9 3 • 9 4 (ABQ t J Λ B = =) L 6, Δ, = 58, 2 H), 5 • 2 3 (d »J = 9 1 H) &gt; 5 • 4 2 (d &gt; J = 1 1 t 1 Η) 9 7 * 1 a 7 • 5 (m 1 6 H) O 13 C-NMR (δ »CDC 1 3, TFA) • # 2 1 • 0» 2 7 • 9 $ 3 8 * 8 »3 8 .9, 4 5 .7, 4 8 • 2» 5 2 • 5 f 6 1 4 9 6 4 .6, 1 2 2. 2 The paper size is in accordance with China Sleepy Family Standard (CNS) A 4 specifications (210 X 297 mm) _ Ο〇5 A6 B6 V. Description of the invention (203), 125. 7, 126. 6, 127. 2, 128. 9, 129.3, 130.0, 133.5, 135.2, 137. 4, 139. 7, 144. 0, 156. 4, 169.3, 1 7 6. 〇0 IR (cm_i, KBr): 1660 (width, C = 〇) Ο FAB MS (%): 561 (parent +1, 44), 488 (34), 408 (28), 207 (67) , 1 5 7 (1 0 0) 〇 Analysis and calculation of C32H37N4O3C 1 · 1 / 4Η2〇: C 67.95, Η 6.68, Ν 9.91. Experiment: C 68.12, Η 6. 4 7, Ν 9. 5 2 〇

1 Example Η Q Shunyi 1— (第 Η 丁丁华 acetamide) —3 1—Zhu Ji swollen—1) 5 —Benzylic 1 7 — (3 —methyl Rongji) Six krypton

H Printed by Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the precautions on page f and then this page) i installed. — (Made in accordance with the method of Example 60 by Zishun 11 (third butylacetamide) 1 3 Monoamine 5-Phenyl 7- (3-Tolyl) Hexazazepine-2-one one 56% yield, Μ.P. 252-254C. ^ -NMR (δ, CDCla, TFA) : 1. 2〇 (single peak, 9H), 2 · 0 — 2.4 (multiple lines, 4H), 2. 3 2 (s, 3 Η), 2. 3 3 (s, 3 Η), 3. 2 7 (m, 1 Η), 3.9 9 3 (AB &lt; r, J ι this paper ruler ^ Applicable to China National Standards (CNS) A 4 specifications (210 X 297 mm) 206 A6 B6 Employee consumption of the Central Standards Bureau of the Ministry of Economic Affairs Printed by the cooperative. V. Description of Invention (〇4), Λ, = 54, 2 Η), 5. 20 (d, J = 9, 1 H), 5.38 (d, J = 1 1, 1 H), 7. 0-7. 5 (m, 1 6 H) 73C ~ NMR (δ, CDC13, TFA): 2 1. 1, 2 1. 2, 2 8. 0, 3 8. 7, 39.0, 45. 8, 48. 3, 5 2. 6, 61. 6, 1 2 0.4, 1 2 4. 2, 126.4, 1 2 6. 7, 1 2 7. 2, 127.5, 128.9, 1 2 9. 2 , 129.7, 1 3 0. 1, 1 3 0. 2, 135.3, 136.5, 1 3 9. 2, 1 4 0. 2, 144.0, 1 5 8, 1 6 9, 17 5. 6 〇IR ( cm- KBr): 1660 (width, C = 0) o FAB MS (96): 541 (parent +1, 72), 4 6 8 (6 3), 4 0 8 (4 5), 2 5 0 (3 2 ), 2 0 7 (1 0 0), 157 (1 0 0), 119 (6 8) o Analyze and calculate C 4〇3: C 7 3. 3 0, H 7. 4 6, N 10. 36. Experiment: C 73.02, H 7. 3 9, N 10.30. Fen Shi Example 9 0 Shunyi 1— (The third butyl is acetaminophen) —3— (3-Methylhydrocarbazide) —5—dithiol 7— (3—Shenben) Hexaargonium complex 1 2 (Please read the notes on the back before writing this page) This paper scale is applicable to the Chinese National Standard (CNS> A4 specification (210 X 297 mm) -207 Yu. '… A6 B6 Employees of the Central Standards Bureau of the Ministry of Economic Affairs Printed by the consumer cooperative V. Description of the invention (205) The ketone was prepared from cis-1— (third butylacetamide) —3-amino—5-phenyl-1--7 (3-tolyl) according to Example 60. Hydrazine leather 2-one ketone 7 6 • 5% yield of amorphous solid ketone Ο 1 Η--NMR (δ, CDC 1 3, τ FA) • 1 • 1 9 (single peak $ 9 H) 9 2 • 0 — 2 • 4 (multi-line f 4 H) 9 2 • 3 2 (s »3 Η) 9 2 • 2 8 (mf 1 Η) t 3 • 8 1 (s 9 3 Η) 9 4 • 0 (m, 2 H) t 5 • 2 1 (dt J = 9 9 1 Η) &gt; 5 • 3 9 (d parameter J = 1 1 t 1 H) &gt; 6 • 7 — 6 • 9 and 7 • 1 — 7.4 (m »1 6 H) 〇13 C — N Μ R (δ» CDC 1 3, TFA) 4 «2 1 • 1, 2 8 • 〇t 3 8 • 8 9 3 9 • 1» 4 5 • 7 9 4 8 • 2 * 5 2 ♦ 6 t 5 5 • 4 t 6 1 • 6 f 7 1 • 0 »1 2 6 • 4» 1 2 6 • 7 t 1 2 7 .2 »1 2 8 • 9 t 1 2 9 ♦ 2 9 1 3 0 • 1 t 1 3 0 .5 9 1 3 6 • 6 t 1 3 9 • 2 t 1 4 4 • 1 t 1 5 7, 1 6 9 f 1 7 6 OIR (C m -1 IKB Γ) • 1 6 6 0 (width »C = 0) 〇FAB Μ S (%): 5 5 7 (parent + 1 t 3 4) 9 4 8 4 (3 9) 9 4 0 8 (3 2), 2 0 7 (7 5) 1 1 9 (1 0 0) 9 1 0 3 (1 0 0) 〇 Analysis and calculation C 3 3 Η 4 0 N 4 0 4 ♦ H 2〇: c 6 8. 9 7 t Η 7 • 3 7 t Ν 9 • 7 5 〇 Experiment * • C 6 8 «7 3 9 Η 7 • 9 5 (一 0 5 8) &gt; N 9 4 2 〇 (please read the precautions on the back before filling in this page) This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -208 Fen ,. . A6 ____B6_ V. Description of the invention (206) Endeavour Example 9 1 鈑 一 1 1 (third butyl ethyl tyramine) a 3 — (3 — argonyl urea) a 5 — Rong a 7 — (3 — Jia Rongmou) Hexahydrogen 31- 2 —

1L According to the method of Example 60, it was prepared from cis-1-1- (third butylacetaldehyde amine) -3-amino-5-phenyl-1-7- (3-tolyl) hexahydroazazepine ~ 2-ketone 6 5 % Yield of amorphous solid. (Please read the precautions on page f before writing this page) Printed by the Central Standards Bureau of the Ministry of Economic Affairs Xinggong Consumer Cooperatives 2 Η--NMR (δ, CDC 1 3 &gt; TFA) • • 1 ♦ 2 0 (BO Zaofeng * 9 Η) »2 • 0 — 2« 4 (multi-line 4 H) »2 • 3 3 (s 9 3 H) 9 3 • 2 9 (m 9 1 H) f 3 • 9 5 (AB &lt; 1 $ ί Λ a = = 1.6, Δ „= 58, 2 H) • 5 • 2 2 (d 9 J = 9 t 1 H) 9 5 • 4 4 (df J = 1 1 9 1 Η) t 7 • 1 — 7 • 4 (m 9 1 6 H) 0 1 3 C-NMR (δ 1 CDC 1 3, TFA) • 2 1 • 2 t 2 8 • 0 f 3 8 • 8 t 3 9 • 0 f 4 5 • 7 &gt; 4 8 • 2 t 5 2 • 5 t 6 1 • 7 $ 7 1 • 1 9 1 2 5 • 6 9 1 2 6 • 3 i 1 2 6 • 7 9 1 2 7 • 2 t 1 2 8 • 9 9 1 2 9 • 2 t 1 3 0 • 2 t 1 3 0 • 5 1 3 5 # 2 f 1 3 6 ♦ 5 9 1 3 9 • 2 • 1 4 4 • 0 $ 1 5 7 » 1 6 9 t 1 7 6 Ο IR (cm -1 9 KB Γ) • »1 6 6 0 (width t C = 0) ○ FABM s (96) ♦ 5 6 1 (parent + 1 t 3 0)» This paper is again applicable to the China 8 «Home Standard (CNS &gt; A 4 specifications (210 X 297 mm 209 Pack · Order · 7 B6 V. Invention description (207) 4 8 8 (7 5), 4 0 8 (4 3) »2 5 0 (37), 2 0 7 (1 0 0), 1 1 5 (3 9) Ο Analytical calculation C 33h 3 7 Ν 4 0 3 C 1 ♦ 1/4 Η 2〇: C 6 7 • 9 5 9 Η 6 • 6 8, Ν 9 • 9 1. Experiment: C 6 7 • 8 9 9 Η 6 • 7 2, Ν 9 • 9 1 0 Example 9 2 1-(third butylacetamide)-3-12 _ tolyl ureido) B. 7 —Dibenzyl hexafluorohetero-2-keto produced from Example 60 The higher polar amine diastereomer (third butylacetamide) -3-amino-5, 7-diphenyl Hexahydroazepine-2-ketone 26% yield, mp 145-15310. 2H-NMR (δ, CD3SOCD3): 1. 15 (single peak, 9H), 1.9-2. 1 (m, 3H), 2. 17 (s, 3 Η), 2. 6 1 (m, 1H ), 3. 25 (m, 1H), 3. 51 (AB ,, J Λβ = 1 6, D n = 2 1 4 (please read the precautions on the back before filling this page) Staff of the Central Bureau of Standards of the Ministry of Economics Printed by consumer cooperatives Η (3 5 7 * ix 5, ·, m 8 / ι \ \ 1 /, Η 4) 1. Η, 7 1 m-, (88 ο. II 1 6 J 5) d * Η () 1 7 Η, 7 20., 17 8 2 DC ο S 3 · D 7 C 4, fee οο ο / tv R 5 Μ 4 Ν, I 5 9 4, ο d

J Η 1 s 2 5 2,: 9 8 8, 3 ο.. 6 12 2 1 1 *, ο 9.. 6 0 2 2 1 1,, 9 3.. 5 7 2 Co i ± 9 9 4 0 • · 9 2 5 2 This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -210

A6 V. Description of the invention (2〇 ^) 1 2 6 • 7 &gt; 1 2 6 • 8 t 1 2 7 • 2 * 1 2 8 ♦ 0 f 1 2 8 «4 9 1 2 8 • 5 t 1 2 8 • 7% 1 2 9 • 4 f 1 2 9 • 5 negative 1 3 0 • 1 f 1 3 1 • 3 $ 1 3 8 «2» 1 3 9 ♦ 3 f 1 4 6 • 3 • 1 5 4 • 4 t 1 6 7 • 3 &gt; 1 7 3 ♦ 4 〇IR (C m -2 t K Β Γ) • • 1 6 5 0 (width * c rs 0) 0 FAB Μ S (%) • • 5 2 7 (Parent + 1 t 9 0), 4 5 4 (7 5) f 3 9 4 (4 5) 9 1 9 3 (1 0 0), 1 5 7 (6 7) f 1 1 9 (5 4) 9 9 1 (6 6) o Analysis and calculation of C 3 2 Η 3 8 Ν 4 0 3 ♦ 1/2 Η 2〇: C 7 1 ♦ 7 5 »Η 7 ♦ 3 4 t Ν 1 0 • 4 6 o Experiment: c 7 1 ♦ 8 4 »Η 7 * 1 0 t Ν 1 0 2 7 O ------ installed ------ ordered (please read the precautions on the back before filling in this page) Central Standard of the Ministry of Economic Affairs Printed by the employee consumer cooperative of the bureau. Example 9 3 1 1 f 1 flute tributyl acetamide) 1 3 — (4 1 atmosphere Rong certain urea) 1 5. 7 — 2 Rongji six gas 氤 miscellaneous rice — 2 — The ketone was prepared from Example 60. The higher polar diastereomer 1- 1 (third Amine-yl acetaldehyde) a 3-amino-5, 7-phenyl-hexahydroazepin a leather -2-one 19% yield, mp 165 - 170¾. 2 Η-NMR (δ, CDC 1 3, TFA): 1. χ g (single peak, 9H), 2.03 (m, lH), 2.2 — 2. 4 (m, 2H), 3. 28 (m, 1H ), 4. (AB «, Jab = 1 7, Dn = 132, 2H), this paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs System A6 B6 V. Description of the invention (20 $ 5.26 (δ, J = 9, 1 Η), 5.43 (δ, J = ll, 1H), 7.1-7.4 (m, 17H) 〇i3C-NMR (δ, CDCla, TFA): 27. 7, 38. 5, 3 8. 6, 45. 7, 4 8. 1, 5 2. 9, 53. 7, 61. 9, 71. 6, 124. 7, 1 2 6. 5, 1 2 7. 3, 1 2 8. 7, 1 2 8. 9, 12 9. Ο, 1 2 9. 4, 129.6, 129.7, 129.8, 130.0, 1 3 3. 6, 1 3 6 . 2, 1 4 3. 6, 1 5 7. 4, 169.8, 176.3. IR (cm-2, KBr): 1650 (width, C = 0) Ο FAB MS (96): 547 (parent +1, 23), 4 7 4 (2 2), 420 (1 5), 3 9 4 (1 6), 193 (2 8), 155 (4 5), 136 (3 0), 119 (100), 104 ( 40) 〇

Analysis and calculation 〇32 ^^ 51 ^ 4〇3 (: 1 · 1 / 2Η2〇: C

6 6. 9 6, Η 6. 5 2, Ν 10. 07. Experiment: C 66. 65, Η 6. 3 3, Ν 9.86. Fen Shi Example 9 4 1 one (the third butyl acetamide) one 3 — (5 — (Rong and three brain base) one 5.7 — two Rong argon xenon complex leather one 2 — ketone equipped with N2 inlet And 35111) 2 round bottom flask of the condenser, add 62mg (0.282mm〇l) benzotriazole mono 5-bag of acid, 5mi (please read the precautions on the back before filling this page). Pack · Order. This The paper scale is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -212 A6 B6 V. Description of the invention (210) anhydrous tetrahydrofuran, 0. 0 9 0 mi (Ο. 4 2 0 · «» 〇1 ) Diphenyl magnetic leaven gas, and 0.060 mi? (0.420 * 〇1) Triethyl press. The reaction was refluxed for 1 hour, cooled briefly, and added 150 min: (0 · 3 8 2 ·· 〇1) 1 — (third butylacetamide)-3-amino- 5,7_diphenylhexahydrogen Azazema 2-heir (the higher diamine diastereomer of Example 60) and refluxed for 14 hours. The reaction was cooled, filtered to remove a small amount of amide by-product that had formed, and the filtrate was evaporated to dryness. The residue is (please read the note on the back of the item first and then «write this page >> The Ministry of Economic Affairs Central Standards Bureau W Industrial and Consumer Cooperatives printed gas imitation milling to produce a white solid t 7 〇mg (34%) tm P 2 1 0 1 2 2 0 V 〇2 H--NMR (δ, CDC 1 3) • 1 • 1 6 (single peak, 9 Η) »2 • 0 3 (mt 1 H) 9 2 • 2 — 2« 5 (m, 3 Η) 9 3 • 1 8 (m »1 H) 9 3 • 2 8 (mt 1 H)» 4 • 0 1 (AB q, J Λ B =: L 6, D n = 10 8, 2 H) &gt; 5 »2 — 5 • 3 (m» 2 H) »5 • 6 4 (bs 9 1 Η) t 7 • 1 — 7 • 4 (m» 1 3 H) t 7 ♦ 9 2 ( d 9 J = 9 * 1 H) 9 8 • 0 6 (s »1 H) t 8 • 3 8 (S i 1 H) 0 1 3 C — NMR (δ * CDC 1 3): 27. 9, 3 8 • 6 t 3 9 ♦ 0 t 4 5 * 6 t 4 8 • 0 9 5 2 • 5, 5 3 • 4 t 6 1 • 8 »1 1 6 • 1 9 1 1 9 • 9 9 1 2 5 ♦ 2 t 1 2 6 • 5 t 1 2 7 • 4 * 1 2 8 • 9 9 1 2 9 ♦ 5 9 1 2 9 »7 t 1 2 9 • 9 1 3 0 ♦ 5 f 1 3 5 • 0 9 1 3 6 • 3 t 1 4 0 • 9 »1 4 3 • 7 &gt; 1 5 5 1 f 1 6 3 • 0 t 1 6 9 • 2 1 7 5 • 8 o-Binding · Order · This paper scale is applicable to 8 National Standards (CNS) A 4 specifications (210 X 297 mm) A 213 A6 B6 _ 5. Description of the invention (feu) (Please read the precautions on the back before writing this page) IR (cm'S KBr): 1640 (Wide, C = 0) o FAB MS (96): 555 (Parent +1, 64) , 481 (70), 394 (35), 193 (83), 155 (55), 119 (100) 〇HRMS: calculation 〇ηΗ36Ν7〇3: 554.2872. Experiment: 554. 28607. Fen Shi Example 9 5 1— (Third butyl acetamide) —3— (3.4. Dimethylbenzyl urea) —5.7.—Dirong a six-gas xenon mixed leather—2-ketoyi Example 94, Use Example 60 The higher-polarity isomer 1- (third butylacetamide) -3-amino-5,7-diphenyl-hexahydroazazepin-2-one produced 48% Rate, mp 185-188¾. 'H-NMR (δ, CDC13): 1. 19 (single peak, 9H), 2.0 (m, lH), 2.14 (s, 3H), 2. 15 (s, 3 Η), 2. 2-2. 3 (m, 2 Η), ο 2 3 Printed by the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economy H 8, H 13) 1, .H, 0 L〇1 s1, * b-) 6 (H, J Η II 3 1 4 * 1 J 5, B d,,. M A (od 7 ((61 (, 591 »1) 5 5. 7 7 H. · 5 II. 3 2 3, J 6 1 m

B A J

6 1X

η D 7 s H2H 7 9-, 5, ο 3 4 Η 2 ddm ✓fv 4 o 9 rH Jc Dc δ / (VRMN -c -214 This paper scale applies the Chinese National Standard (CNS) A 4 specifications (210 X 297 Mm> Α6 Β6 V. Description of the invention (212) 19.9, 28.6 4 8. 2, 5 1. 1, 12 1.8, 12 12 7. Ο, 128 12 8. 9, 129 13 6. 8, 137 15 5. 4, 167 IR (cm called, 39.3, 39.4, 46.1,, 52.2, 61.2, 117.9 1. 9, 1 2 6. 5, 1 2 6. 6, .5, 128.6, 128.8, .4, 129.5, 130.0, .1, 138.2, 145.3, .5, 17 5. Ο 〇Κ Β r): 1660 (width, C = 0) (please read the precautions on the back before filling this page) 1 FAB MS (%): 541 (48, parent + 1), 468 (3 5), 394 (32), 3 0 9 (3 9), 193 (4 2), 155 (100), 1 3 5 (7 2), 119 (1〇〇), 1〇 3 (96) ○ Analysis and calculation of C33H4〇N4〇3: C 73.30, Η 7.46, N 10.36. Experiment: C 73.09, Η 7.32, N 10.08.

Example 9 R 1-(The third Ding r sleeps Ban — 3 — (3 —Dishen a certain amine and a gland base) a 5.7 to dizhu a hexahydrogen mixed leather 2 — _ According to Example 94, Use Example 60 The more polar isomer 1- (third butylacetaldehyde amine) -3-amino-5,7-diphenyl-hexahydroazazepine-2-one 7 1% yield, mp 145-153¾. 7H-NMR (δ, CDC13): 1 · 18 (single peak, 丨 installed. Ordered _ Printed by the Ministry of Economic Affairs Central Standard Beigong Xiaozuo Co., Ltd. The paper size is in accordance with China National Standard (CNS) A4 specifications (210 X 297 mm) 215 A6 B6 Printed by the Employees ’Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (213) 9 Η) $ 1 • 9 8 (mt 1 H) 9 2 Φ 2 2 (m 9 2 H ) 9 2 • 5 7 (mt 1 H) »2 • 8 7 (s» 6 H) f 3 • 2 0 (m »1 H) f 3 • 5 8 (ABJ Λ a = 1 6 t D η = 1 7 4 »2 H) t 5 • 1 7 (d $ J = 1 0» 1 Η) 9 5 • 2 6 (mt 1 H) 9 5 • 4 2 (st 1 H) »6 • 3» 6 • 6 9 6 • 7 f 6 • 9 and 7 • 0 a 7 • 3 (mt 1 6 Η) f 7 * 5 9 (s 9 1 H) 〇1 3 C — Ν MR (δ t CD c 1 3) 4 4: 28. 6, 3 9 • 4 »3 9 * 5 f 4 0 • 6 t 4 6 • 0, 4 8 • 3, 5 1 • 1 * 5 2 • 1 9 6 1 • 2 t 1 0 4 • 5 &gt; 1 0 7 * 7 9 1 0 8 • 5 9 1 0 8 • 6 f 1 2 6 • 6 t 1 2 7 • 0 &gt; 1 2 8 • 6 * 1 2 8 • 8 &gt; 1 2 8 • 9 9 1 2 9 • 1 $ 1 2 9 • 3 f 1 2 9 • 5 f 1 3 8 • 3 9 1 4 0 • 1 t 1 4 5 • 3 f 1 5 1 • 5 f 1 5 5 • 3 9 1 6 7 • 5 »1 7 4« 9 0 IR (cm -1 f KB Γ) • • 1 6 4 〇 (width * C = 0) 0 analytical calculation C 3 3 H 4 1 N 5 0 3 1/2 H 2 0: C 7 0 • 1 9 H 7 • 5 0 9 N 1 2 • 4 0 0 Experiment: c 6 9 * 8 1 H 7 • 1 3% N 1 2 • 0 5 o salt The acid salt is formed in ether with HC 1 and crystallized from acetone to produce a white solid 9 m P 1 9 0 — 1 9 7 t: o Analytical calculation C 3 3 H 4 l N 5 0 3 Η C 1: C 6 6 • 9 3, Η 7. 15, Ν 11. 83. Experiment: C 66.60 (please read the precautions on the back before filling in this page) 1-Pack · The paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) 216 Α6 Β6 V. Description of the invention (214 ), Η 7. 1 7, Ν 11.70. Fu Shi Example 9 7 Shun Yi 1 1 (the third butyl ethyl amine) a 3-(3-methyl urea urea) a 5-Rong a 7-(3 —Methylargon) Hexaargon Xenon Heterochloride 2-keto (please read the precautions on the back before filling in this page) The same example 6 0 is printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. Compound 1 mono (third butylacetaldehyde amine) — 3 — amino group — 5 — phenyl mono 7 — mono (3 — methyl gas phenyl) hexahydroazepine 2 — ketone 4 0 96 yield, m P 2 4 5 — 2 4 7 Co 2 Η--NMR (δ, CDC 1 3 »TFA) • 1 • 19 (aa early peak t 9 Η) f 1 • 9 — 2 • 4 (multiline t 4 Η) t 2 • 3 3 (sf 3 Η) f 3 • 2 8 (m 9 1 H) I 3 • 8 1 (s 9 3 Η) t 3 • 9 7 (AB 4 9 J λ Β ~ =) L 7 f D η Y ο Γ k = 6 2 f 2 H) f 5 • 2 3 (df J = 1 0 9 1 Η) $ 5 • 3 8 (d »j = 1 1 1 Η) t 6 • 8 —— 7 • 4 (mt 1 6 H) O 13 C — Ν Μ R (δ t CDC 1 3, TFA) 2 1 • 〇f 2 7 «9 * 3 8 4 6 t 3 8 • 8» 4 5 • 6, 4 8 • 2 t 5 2 • 8 9 5 2 • 9 f 5 5 • 5, 6 1 ♦ 6, 1 1 4 • 7 »1 1 5» 9 9 1 2 1 • 9 t 1 2 4 • 5 t 1 2 6 • 6% 1 2 7 • 3 f 1 2 8 • 0 »1 2 8 • 9 9 1 2 9 • 7 * 1 3 0 • 5, 1 3 8 • 0 f 1 4 0« 3 1 4 3 • 8 f 1 5 8 t 1 6 9 »1 7 5 • 6 o IR (cm'2, KBr): 1650 (Wide, C = 0) i Pack · Order _ This paper scale is applicable to China's Sleepy Family Standard (CNS) A 4 specifications (210 X 297 mm) -217 A6 Central Standard of the Ministry of Economic Affairs Printed by the Bureau ’s Consumer Cooperatives _B6_ V. Description of Invention (215) 〇FAB MS (96): 557 (Parent +1, 30), 4 8 4 (4 5), 2 6 6 (3 0), 2 2 3 (1 0 0), 132 (45), 114 (42), 91 (44). Analysis and calculation C33HmN4〇4: C 71. 20, Η 7. 2 4, Ν 10. 07. Experiment: C 70. 98, Η 7. 5 1, N 9.83. Fen Shi Example 9 8 Shunyi 1 I (Zuo butyl acetamide) a 3 — (3 — methyl argon and a certain urea) a 5 — Zhu Ji a 7 — (3 — methyl argon Zhu) hexahydroxenon Leather 2-ketone The same as Example 60, prepared from the higher polar isomer 1_ (third butylacetamide)-3-amino-5-phenyl-7-(3-methylphenyl) hexahydro Azazema 2-keto is an amorphous solid with a 46% yield. ^ H-NMR (δ, CDC13, TFA): 1. 19 (please read the precautions on the back before filling in this page) (αο 早 峰> 9 H) »2 • 0 1 2» 4 (multiline, 4 Η), 3 »2 9 (m ♦ 1 H)» 3 8 0 (s, 3 Η), 3 • 8 2 (s 9 3 H) »3 • 8 — 3 .9 and 4.0-4 • 1 (mt 2 H) 9 5 • 2 5 (m ， 1 Η), 5.38 (mt 1 H) t 6 • 7 — 7 • 0 and 7. 1-7 .4 (m, 1 6 Η) O 13 c- NMR (δ &gt; CDC 1 3, TFA) • 2 2. 1,28.0, 38.7, 38.8, 45.6, this paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -218 A6, Guang -_ B6 V. Description of the invention (216) 47, 52, 55. 4, 55 · 5, 61. 5, 114. 6, 115.8, 121.7, 126.6, 127. 2, 128. 9, 130 · 5, 143.9 (the remaining masters are not shown in this scan). IR (cm · 2, KBr): 1670, 1630, 1600 (width, C = 〇) ○ FAB MS (96): 573 (parent +1, 45), 5 0 0 (5 2), 4 2 4 ( 35), 266 (3 4), 2 2 3 (1 0 0), 132 (3 2), 115 (48), 9 1 (37) 〇 analysis calculation C 5 ♦ H 2〇: C 67.10, H 7. 1 7, N 9.48. Experiments: c 6 7.01, H 7. 2 3, N 9.20o Late night 9 9 Shun —! — F flute tributyl acetamide) a s one (3 — gaseous urea group) a 5-benzine One 7-(3-A gas method) six atmosphere mixed leather one 2

—BpI Printed by R Industry and Consumer Cooperatives, Central Bureau of Standards, Ministry of Economic Affairs (please pay attention to Mnwe first and then write this page). Made from the higher polar isomer 1-1-1 (third butylacetaldehyde) as in Example 60 ) A 3-amino- 5-phenyl- 7- (3-methyl gas phenyl) hexahydroazepine 2- ketone 31% yield of amorphous solid. 1 Η-NMR (δ, CDC 1 3, TFA): 1.20 (single peak, 9H), 2.0-2.4 (multiple lines, 4H), 2.33 (s, 3H), 3.29 (m, lH ), This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -219 5. Description of invention (217) A6 B6 Printed by the Employees Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 3 • 8 1 (s » 3 H) f 3 fight 9 6 (AB 9 t J Λ B =) .7 »D η = 5 9 9 2 H) 9 5 • 2 4 (dt J = 9 9 1 Η) 9 5 • 4 2 (d »J = 1 1 9 1 Η) t 6 • 8-7 * 4 (m 9 1 6 H) o 13 C — NMR (δ t CDC 1 3, TFA) • • 2 2 f 2 8« 0 &gt; 3 8 • 7 f 3 8 • 8 »4 5 • 6 4 8 • 2 9 5 2 • 5» 5 5 • 4 $ 6 1 • 6 $ 1 1 4 .7 9 1 1 5 • 9 »1 2 1 • 8 , 1 2 5 • 8 9 1 2 6 * 6, 1 2 7 • 2 t 1 2 8 * 9, 1 3 0 • 5 9 1 3 0 • 6 »1 3 8 • 1 t 1 4 3 • 9 f 1 5 6 9 1 6 7 t 1 7 5 Ο IR (cm -1> κ B r) • • 1 6 7 0 9 1 6 2 0, (width * c = 0) OFABM s (%) • 5 7 7 (Parent + 1 t 3 5), 5 0 4 (4 6) t 2 2 3 (1 0 0) f 1 5 7 (7 3), 1 1 9 (5 1) 0 Analytical calculation C 3 2 H 3 7 N 4 0 4 C 1 ♦ H 2 0:: C 6 4 • 5 8 9 H 6 • 6 0 9 N 9 »4 1 0 experiment • • C 6 7 • 5 4 H 6 • 6 3 t N 9 • 2 4 0 Elite case 1 0 0 cis 1 (third τ Hua acetamide) 3 (3 Tolylurea &) _ 5 Benzene cap 7 (4 _ Sanqi JL Huabenhua) —JL * Radon 护 azaine-2 — Manufactured from the same as in Example 6 Hexahydroazepine leather 2 —The paper standard of ketone third butylacetate is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -220 (please read the precautions on the back before writing this page) A6 B6 V. Description of the invention (218) Amorphous solid with 10% yield of amine. 2H-NMR (δ, CDC13, TFA): 1.19 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before writing this page) (Single Peak 9 9 Η) 9 2 • 0 1 2 • 4 (multiple wire 9 4 H) 9 2 • 3 4 (s »3 H) f 3 • 3 1 (m 9 1 H) f 3 • 8 2 (ABQ t J a B = ί 6, D n = 3 Θ t 2 H) $ 4 • 8 2 and 5 • 0 2 (mt 1 H) »5 * 3 (mt 1 H, 7 • 0 — 7 • 7 (m 9 1 6 H) o 1 3 C — NMR (δ »c DC 1 3, TF 'A) 2 1 • 1 t 2 8 • 〇» 3 8 • 6 t 3 8 • 8 9 4 3 • 3 4 5 • 6 9 4 8 • 4 »5 2 • 7 t 6 1 • 0 9 1 2 0 • t 1 2 1 • 2 f 1 2 4 • 4 t 1 2 5 • 0 »1 2 6 • 2 1 2 6 • 5 9 1 2 6 • 6 9 1 2 6 • 9 t 1 2 7 • 3 f 1 2 7 • 7 t 1 2 8 • 2 9 1 2 8 ♦ 9 f 1 2 9 • 7 f 1 3 0 • 0 t 1 3 1 • 5 f 1 3 1 • 9 t 1 3 4 ♦ 8 f 1 3 5 • 0 t 1 4 0 • 3 $ 1 4 〇 • 5 t 1 4 3 • 7 t 1 4 3 • 9 t 1 5 8 t 1 6 8 »1 7 5 〇IR ( C m -1 1 KB r) • • 1 6 8 0 t 1 6 6 0 f 1 6 4 0 (width tc = 0) O FABM s (%) • • 5 9 5 (parent + 1 9 5) f 4 8 2 (2 4) 9 3 4 9 (3 0) »1 5 7 (1 0 0) 1 3 5 (4 5) f 1 1 9 (9 9) 9 1 0 3 (5 1) 〇Analysis and calculation C 3 3 H 3 7 N 4 0 3 F 3 .3 /, 2 H 2 0 • c 6 3 • 7 5 t H 6 4 9 »N 9 0 1 0 experiment • Φ c 64. 01, Η 6. 4 4, N 8.74. This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -221 A6 B6 V. Description of the invention (219) Example 101 Shunyi 1 1 (the third butylamine) 3 — ( 3 —Shen Juzhu urea group) —5 —Stupyl group 7 _ (4 —Trihydromethyl carbazide) hexacyanoxenon leather—2 —brewed from the higher polar isomers in Example 60 1 A (third butyl acetamide)-3-amino-5-phenyl-7_ (4-trifluoromethylphenyl) hexahydroazazepine-2-one 48% yield of amorphous solid . &quot; H-NMR (δ, CDCla, TFA): 1. 18 (please read the precautions on the back before writing this page) Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (single peak 9 9 Η) f 2 • 0 1 2 4 (multiline f 4 H) »3 • 3 1 (m 9 1 H) t 3 * 8 2 (st 3 H)» 3 • 8 3 (AB 4 »J Λ B = 1.6, D n = 3 7, 2 H) 9 4 • 8 2 and 5 • 0 2 (m 9 1 H) f 5 • 3-5 • 4 (m 9 1 Η) »6 • 7 — 7 * 7 (mf 1 6 H) 0 1 3 C-NMR (δ, CDC 1 3, TFA) • 2 2 • 1 t 2 8 • 0 t 3 8 • 5 t 3 8 • 7 9 4 3 • 3, 4 5 * 6 9 4 8 • 4 p 5 5 • 5 t 6 0 • 9 9 1 2 6 • 2 f 1 2 6 • 5 f 1 2 6 «6 t 1 2 6 • 9» 1 2 7 ♦ 3 t 1 2 8 ♦ 9 t 1 3 0 • 1 f 1 3 0 • 6 9 1 3 0 • 8 9 1 4 0 • 5 9 1 4 3 • 7 9 1 4 4 • 0 9 1 5 7 • 7 9 1 6 8 9 1 7 6 〇IR (cm -1 9 KB r) «♦ 1 6 6 0» 1 6 4 0 9 1 6 6 0 (width> c rs 0) O FAB MS (%): 611 (parent +1, 4), installed _ Order · -222 This paper scale is applicable to China's national standard CNS) A 4 size (210 x 2 mm Ding> A6 B6 five, description of the invention (220 &gt;

4 9 8 (1 7), 3 4 9 (2 0), 157 (1 0 0) 〇 Analysis calculation C33H37N4〇4F3 · Η2〇: C 6 3 0,5, Η 6. . Experiments: C 6 3. 0 5, Η 6. 1 1, N 8. 5 9 〇 Fen Shi Example 1 0 2 cis-1 1 (tributyl acetylamine)-3-(3-atmosphere Benzylurea ) —5-benzyl-7- (4-digasomethylphenyl) hexagas gas leather-2 is prepared from the higher polar isomer 1-1- (third butylacetaldehyde) as in Example 60 ) A 3-amino-5-phenyl- 7- (4-trifluoromethylphenyl) hexahydrocyanide 2- 2-one amorphous solid in 34% yield. 'H-NMR (δ, CDC13, TFA): 1.19 (Please read the precautions on the back before filling in this page) Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (tao Zaofeng f 9 Η), 2 • 0 1 2 • 4 (multiline> 4 H), 3 • 3 3 (mt 1 H) 9 3 • 9 3 (AB 9 t J Λ b = 1 7 9 D η = 8 9 f 2 H) t 5 • 3 7 (m minus 1 H) t 5 • 4 6 (dt J = 1 1 9 1 H) t 7 • 0 — 7.7 (mf 1 6 Η) Ο 1 3 C-NMR (δ »c DC 1 3 , TFA) • 2 7 • 8 9 3 8 • 6 t 3 8 • 7 t 4 5 • 6 »4 8. 3, 5 2 • 6 t 5 3 • 1 t 6 1 • 1 t 1 2 0 • 4 9 1 2 2 • 6 t 1 2 6 • 2 t 1 2 6 • 6 9 1 2 7 .4, 1 2 9 • 0 f 1 3 0 * 0 t 1 3 0 «6 t 1 3 2 .〇, 1 3 5 • 3 9 1 3 7 0 9 1 4 0 • 3 9 1 4 3 .6, this paper scale is applicable to Zhongpu® Home Standard (CNS> A 4 specifications (210 X 297 mm) -223

Α6 Β6 5. Description of the invention (221) 1 5 7 $ 1 6 9, 1 7 6 «1 Ο IR (C m -1 9 Κ Β Γ) • 1 6 8 0 9 1 6 4 0 (width f C = 0 ) FAB M S (96) ♦ 6 1 5 (parent + 1, 6) f 2 3 3 (2 3), 1 5 7 (1 0 0) 9 1 3 5 (4 7) 9 1 1 9 ( 9 9), 1 0 3 (5 2) Ο Analytical calculation C 3 2 Η 3 4 Ν 4 0 3 C 1 F 3 • 5/4 Η »0 • c 6 0 • 2 8 t Η 5 ♦ 7 7 I Ν 8 • 7 9 Ο Experiment • • C 6 0 • 1 7 f Η 5 • 9 1 See Ν 8 ♦ 6 4 0 Example 1 0 3 cis 1-(third butyl ethyl amine) 3 3 even) -5-July-7-(3-gas phenyl) hexahydro scandium oxazin-2-one prepared from the same as Example 60 higher polar isomer 1-(third butylacetamide)-3- Aminyl 5-Phenyl_ (3-Gabenji) Baqi Gas 2-Ketone 39% amorphous solid with a yield of 9%. 2 Η-NMR (δ, C Ό C \ a, Τ FA): 1 · 22 (please read the precautions on the f page first and then f this page)-Printed by the Ministry of Economic Affairs Central Standard 4 printed by the employee consumer cooperative 2 3 5 1 Η 9 f peak single Η 4, multiple line weights / ν 4 2 1 ο 2 8 2 • 3 f Η 3 fs / ί. 3 3 B, A d / ΙΛ / i \ 7 1 82 7 R, M) N Η I 1C 3 • i Η 1

Η 2 3 4 II η D, 6 U a A J 9 0 5

H

4C .D 7C (H 2 6 3 1

A F T d

J This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 2 £> 7 Gongmeng) -224 _ V. Description of the invention (77?) 2 1 • 2 f 2 8 .1 t 3 8 • 8 9 3 8 • 9 9 4 5 ♦ 7, 4 8 • 3 9 5 2 .6 t 6 0 • 8 t 1 2 6 • 7 $ 1 2 7. 3 t 1 2 8 • 9, 1 2 9 • 6 9 1 4 4 • 0 t 1 5 7 t 1 6 7 »1 7 5 (not all masters are seen in this scan) o IR (cm -IKB r) • 1 6 6 0 t 1 6 4 0 (width 9 C 0) 〇FABM s (%) ♦ 5 4 5 (Parent + 1 $ 6 2), 4 7 2 (5 2), 2 1 1 (7 6) »1 5 7 (1 0 0), 1 3 2 ( 5 3), 1 0 7 (5 3) t 9 1 (5 7) o (Please read the precautions on the back before writing this page) 丨 Install-

Analysis and calculation C32H37N4〇3F ♦ 3 / 4H2〇: C 6 8.8 6, H 6. 9 5, N 10 .0 4. Experiments: C 6 8. 8 7, H 6. 8 3, N 9. 7 3 〇 Printed by the Central Ministry of Economic Affairs Tong Bei Gong Consumer Cooperatives Example 1 0 4 cis 1 1 (third butylacetamide) ) A 3 — (3-methylphenyl phenyl mianmou) a 5-juju 7 — (3-argon Rongmou) six argon xenon mixed leather 2

-I Prepared from Example 60 Higher polar isomer 1- (third butylacetamide) 3-amino-1 5-phenyl-7- (3-fluorophenyl) hexahydroazazepine-2 -Amorphous solid with 30% yield of ketone. ^ -NMR (δ, C Ό C \ 3t TFA): 1.20 (single peak, 9H), 2.0-2.4 (multiple lines, 4H), 3.28 (m, lH), 3.80 (s, 3H), 3. 9 (m, 2 H), 5. 23 (d, J = 1 1, 1 H) This paper scale is applicable to the Chinese National Standard (CNS> A 4 specifications (210 X 297 mm) -225 order. 9 00 Λ 2

AB Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (223) &gt; 5 • 3 4 (dt J = 1 1 9 1 Η) »6 • 7 1 6 • 9 and 7 • 1 1 7 • 4 (mf 1 6 Η) Ο 13 C-Ν Μ R (δ f CD c 1 3, Τ FA) • • 2 2 • 2 9 2 8 • 2 $ 3 8 • 8 9 3 8 • 9 f 4 5 • 7 »4 8 • 3 9 5 2 • 5 9 5 5 • 4, 6 0 • 8 f 1 1 6 • 5 t 1 2 6 • 7 9 1 2 7 • 2 t 1 2 8 • 9 9 1 4 3 • 9 9 1 7 6 (not all masters are seen in this scan) Ο IR (C m -2 * K Β Γ) • 1 6 7 0 &gt; 1 6 4 0 (width 9 C = 0) 〇FAB Μ S (%) • • 5 6 1 (Parent + 1 t 9 5) t 4 8 8 (7 8) t 2 1 1 (1 0 0) f 1 5 7 (8 9) t 1 1 9 (8 8) o Analysis and calculation C 3 2 Η 3 7 Ν 4 0 4 F 1/2 H 2 O 3: C 6 7 • 4 7 »Η 6 • 7 2 N 9 • 8 3 o experiment • • C 6 7 • 20, Η 6. 7 0, N 9 · 1 4 (--o. 6 9) 〇Η R Μ S calculation C 3 2 Η 3 7 N 4 0 4 F • • 5 6 1 • 2 8 6 8 〇 Experiment • 5 6 1 • 2 8 5 5 2 0 1 Example 1 Q 5 cis 1 (the third τ Hua amine) 3 (3 atmosphere benzene hua m Hua) 5 «benzene hua 7 (3 _ 氲 New) Argon gas 2 Awakening_Manufactured from Example 60 Higher Polar Isomer 1-Mono- (T-Butylacetamide) Mono-Amino-5-Phenyl-7- (3-Gasophenyl) Hexahydroazepine ( Please read the precautions on the back before writing this page) • Binding. Order. This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -226 A6 B6 V. Description of invention (224) ( Please read the note on the back first and then fill out this page) A 2-ketone 52% yield amorphous hip fixation. 2 Η--NMR (δ, CDC 1 3 &gt; TFA) • 1 ♦ 2 2 (single peak f 9 H) t 2 • 0 — 2 • 4 (multiple line t 4 H), 2 • 3 3 (s &gt; 3 H) f 3 • 2 9 (m »1 H) f 3 • 9 (m $ 2 H) t 5 • 2 6 (dt J = 1 1 9 1 H) t 5 * 4 2 (mt 1 H) 9 6 • 9 — 7 • 3 (mt 1 6 H) 〇I 3 C-NMR (δ 9 CDC 1 3, TFA) ♦ 2 2 • 2 $ 2 8 • 1 t 3 8 • 8 9 3 9 * 0 9 4 5 «6 t 4 8 ♦ 4 f 5 2 • 5 f 6 0 • 9 9 1 1 6 • 6 t 1 2 5 • 1 9 1 2 5 • 4 9 1 2 6 • 6» 1 2 6 • 7 9 1 2 7 • 3, 1 2 8 • 9 t 1 3 0 • 5 9 1 3 0 • 9 f 1 3 1 • 0 t 1 3 5 • 2 9 1 4 3 • 9 f 1 5 7 »1 6 4 9 1 7 5 〇IR (cm -1 t KB Γ) 1 6 7 0 t 1 6 4 0 (width 9 C = 〇) 0 FABMS (%) 5 6 5 (parent + 1 f 5 8) 9 4 9 2 (7 1) 9 2 1 1 (1 0 0) $ 1 5 7 (9 1) t 1 3 2 (5 3) 9 1 1 5 (4 2) f 9 1 (4 9) 〇Analysis calculation C 3 1 H 3 4 N 4 0 3 C 1 F «1/2 H 2〇: C 6 4 • 8 6 t H 6 • 1 4 f N 9 • 7 6 〇Experiment • • C 6 4 • 7 9 t H 5 9 3 t N 9 • 4 2 〇 Printed by the Consumer Standardization Bureau of the Central Bureau of Standards of the Ministry of Economic Affairs 1 0 6 -227 Applicable to China's sleepy family standards (CNS> A4 specifications (210 X 297 mm) V. Description of invention (225) 1— (Third butylacetamide) —3— (3-methyl, 4—ambient, please Cage a urea) a 5. 7-two Zhu six 氲 Μ 蕞 一 2 | respect

Prepared according to the method of Example 94 from Example 60, the higher polar isomer 1-(third I butylacetaldehyde amine)-3 monoamino-5 t 7-phenyl-hydrazine leather 1 1 1 1 2- m 7 0% yield »mp 1 6 8 — 1 7 1 V Ο Re t 1 1 1 1 Η--NMR (δ, CDC 1 3) 1 • 1 9 (single peak, this page 'W 1 1 1 9 Η) 9 2. 0 — 2. 3 (m * 3 H) 9 2 • 2 4 (s, 1 3 Η) »2. 6 2 (m, 1 H) &gt; 3 • 1 7 (m, 1 Η ) 1 1} 3 • 5 8 (A Β &lt;?, J Λ B = 1 3, D n = 2] .2, 2 Η 1 1 1) f 5 • 18 (d, J = 1 1 1 H) &gt; 5 • 2 (m, 1 with l 1 Η) 6. 8 7 (d, J — 7 »1 H) t 7 • 0 — 1 1 7 • 4 (m, 1 5 H), 8 ♦ 0 3 (b S * 1 Η) ο 1 1 1 23C-NMR (δ, CDC13): 20. 1, 3 4 8 2 3 5,, 6 3 • 001 2 5

6 8 2 2 1 ± IX 2 • 8 4, 3 3 .8 fb1X 4 1 f 9 02 • · οι 4 6 Printed by the Employees Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 9 6 2 3 1Χ 1χ 6 6 2 3 6 8 2 2 lx 1χ 9 8 2 3 1Χ 1χ 9 7 3 3

7 8 2 2 IX 9 8 2 3 ix 1Χ 9 4 4 1Χ 1Χ 7 9 2 2 9 5 2 4 1 ± ix 4 0 5 2 width ^ fv ο 4 6 1Χ ο 4 6 .6 5 1 7: 1) 9Γ 6 Β.κ 7, 6 7 1Γη, C 4 (.R 5 I 5 1Λ

C ο Β A (F 8 8 4 7 3% / IV s Μ 4 9 3 1) 6 0 5 3 + 3 generation 9 pro 1 2 2 ο ο This paper scale is applicable to China® Family Standard (CNS) A 4 specifications ( 210 X 297 mm) _ 〇28 A6 B6 V. Description of invention (226) (Please read the precautions on the back before filling out this page) 132 (4 0), 119 (4 7), 115 (4 3), 9 1 (62) 〇

Analysis and calculation C32H37N4〇3C 1 · 1 / 2Η2〇: C 6 7. 41, Η 6.7 2, Ν 9.83. Experiment: C 67. 41, Η 6. 7 3, Ν 9. 7 6 〇 Fen Shi Example 1 0 7 1_ (third butylacetamide)-3-(3-nifediurea)

-5, 7 One diphenyl six gas 氤 miscellaneous leather one ρ I was prepared from Example 6 ◦Higher polar isomer l — (third butylacetaldehyde amine) II loaded with I -3 monoamine-5, 7-Phenyl mono-hydroazazepine — 2-keto S 4% II yield, m Ρ I 8 2-I 8 5 V ο III 7 Η--Ν MR (δ, CD 3 s 0 c D 3) : L. L 5 (order I single peak, 9 Η), I .9 -2 · l (m &gt; 3 Η), 2 6 3 III (m, l Η), 3 .3 (m, l Η) 9 3 • 5 2 (A Β QI l, JA Β = l 6, D η = 2 2 8 t 2 H) $ 5 .l 3 (printed by the employee consumer cooperative of the Central Standards Bureau of the Ministry of Economic Affairs

, 817 3 0 2 4 6 II. D. 1 1 1 J 8 Co »».., 〇 ♦ 5 8 2 8 d)) δ,... (HH (0693 2 5 1 R · 2 3 5 31 » M 7 · 1 1 1. S N 4,,,, 5 m (_ * 442 * (6 c 9...) 7 513 · 6 9 8 H 4 2 2 4 1X791 ± 1i 1X 1 s / —X 14 1 5 Η 6 9 D cos 5 5 8 2 Η ix 5 4,.. 7 8 9. 2 5 8:, 2) 61 &gt; ο 2 1 • · 6 3 4 7 1χ This paper size is applicable to Chinese national standards ( CNS) A 4 specifications (210 X 297 mm> -229: 166〇, 1640 (width A6 B6 V. Description of the invention (227) IR (cm, KBr, C = 0) 〇FAB MS (%) 5 5 8 (parent + i, 2 〇), 485 (23), 193 (67), 155 (52), 135 (35), ii9 (i〇〇), i〇3 (48), 9 1 (39 ) 〇

Analysis calculation C3iH35Ns〇5 · 2 /: C

6 5. 3 6, H 6. 4 3, N 12.29. Experiment: C 6 5. 0 6, H 6. 3 5, N ll.g! (Please read the precautions on the back before writing this page) i installed · hard work example 1 0 8 booked. 1 二 丄 第- II ·. Butylacetamide) 1-1 ^ ~ ^ J: 3-amine urea urea) 5.7-diphenyl hexamethylene xenon hetero fused 2 prepared from 1 1 (third butylacetaldehyde Amine) mono (3 monoaminophenylureido) _5,7-diphenylhexahydroazazepine__2-one 90% yield, which is 5 equivalents of ammonium formate in ethanol at room temperature 10% The upper rake is present and the original is returned. Ν Ν Printed by the Ministry of Economic Affairs, Central Standards Bureau, 8 Industrial and Consumer Cooperatives Η 9 Η

£ X Η 2 m 7 2 3 (2 6 R -1 Μ ο) Η J ο 3 ΙΑ ^ C 丨 8 D m 6 (c 1 3 peak Γη single ί (8 7 4 1 .2? V * · Β (A 8 (ο 9. 5 4 • f 3), Η) 2 Η, 1 〇, 6 m 1 (118 η 1 D • 9 3 6, 1 5 1Χ 5 Η 1Χ 9ο 1 ± Η 1Χ, S 7 4 5 6) 2 Η .5 ix, 9) m / IV 4 7 I 7 6 9) Η Η 1

S The paper size is applicable to China National Standard (CNS) Grade 4 (210 X 297 mm) -230 2l39〇i- A6 B6

5. Description of the invention (228) 8 • 9 6 (bs 9 1 H) o 1 3 C NMR (δ &gt; CD c 1 3) 4 4 2 8. 6, 3 9 • 0 »3 9« 6 f 4 6 • 1 t 4 8 • 2 9 5 1 • 2, 5 2 • 2 9 6 0 • 4 t 6 1 • 1 9 1 0 6 • 5 9 1 0 9 • 7 &gt; 1 2 6 • 6 »1 2 6 • 9 9 1 2 7 • 0 f 1 2 8 • 4 9 1 2 8 • 6, 1 2 8 ♦ 8 f 1 2 8 • 9 t 1 2 9 • 1 t 1 2 9 • 5 t 1 2 9 • 7 t 1 3 8 • 3 t 1 4 〇 • 4 t 1 4 5 • 3 f 1 4 7 • 3 9 1 5 5 • 4 9 1 6 7 • 6 f 1 7 5 • 1 o IR (cm -I, KB Γ) • 1 6 4 0 (width »C = 0) 〇FABM s {%) • # 5 2 8 (parent + 1 f 8 1), 4 5 5 (5 3) &gt; 3 9 4 (6 9) »1 9 3 (9 4) t 1 5 7 (9 9) &gt; 1 1 9 (1 0 0) o Analytical calculation C 3 1 H 3 7 N 5 0 3 C 1 φ H 2 0: c 6 8 • 2 3 »H 7 • 2 0» N 1 2 • 8 3 0 Experiment: c 6 8 • 7 3 (+ 0 • 5 0) t H 7 • 〇7 t N (please read the notes on the back first Field to write this page) Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 12.43. Fen _ Example 1 Ο 9 1 — (Third butyl ethoxylamine) — 3 — (3 — Ethylamine ethoxyl urea) — 5.7 — Two stupid six gas 氤 璪 箪 一 2-Ketone system From 1-one (third butylacetamide) to 3- (3-aminophenylureido) to 5,7-diphenylhexahydroazazepine to 2-ketone, 70% of the paper produced is applicable China National Standard (CNS> A4 specifications (210 X 297 ;; -231 213901 A6 B6 V. Invention description (229) rate, its pseudo reflux in pyridine for 14 hours to acetic anhydride acetylation, mp Ministry of Economic Affairs Central Standards Bureau staff Printed by consumer cooperatives

1 9 5-2 0 5 ic oi H--NMR (δ, CD 3 S 0 CD 3) • 1 •] .5 (single peak »9 H) f 1 • 8-2 • 0 (mt 3 Η)» 2 • 5 7 (mf 1 H), 3 * 1 7 (m »1 H) &gt; 3 • 5 1 (AB 4» J Λ B = 1.6, D n = = 2 2 8, 2 H) 9 5. 0: L (m 9 1 H) t 5 * 3 〇 (df J = 1 0 &gt; 1 H) f 6 • 7 — 7 • 4 (mt 1 5 H) t 7 • 6 7 (sf 1 H ) &gt; 9 • 0 1 (st 1 H) 9 9 • 8 2 (bsf 1 H) 〇1 3 c — NMR (δ, c D 3 S 0 CD 3) • 2 4 • 0 »2 8 • 5» 4 5 • 1 t 4 7 • 0 Reference 4 9 • 9 »5 1 • 6 t 5 9 • 4 9 1 1 2 • 0» 1 1 2 • 3 t 1 2 6 • 3 9 1 2 6 • 8 »1 2 8 • 0 t 1 2 8 • 1 negative 1 2 8 • 5 9 1 2 8 • 7 1 2 8 • 8 t 1 2 9 • 3 * 1 2 9 • 4 f 1 2 9 • 5 &gt; 1 3 4 • 6 f 1 3 9 • 3 »1 3 9 • 7 f 1 4 0 • 8 1 4 6 • 3 $ 1 5 4 • 1, 1 6 7 • 3 f 1 6 8 • 2 f 1 7 3 • 3 0 IR (cm -1 9 KB r) • 1 6 6 0 9 1 6 4 0 (寛 9 C = 0) o FABM s (%) • 5 7 0 (parent + 1 9 2 5) t 4 9 7 (2 9) t 1 9 3 (4 2) f 1 5 7 (1 0 0) t 1 1 9 (3 4 ) o Analyze and calculate C 3 3 H 3 9 N 5 0 4 ♦ H 2〇: C 6 7. 4 4 f H 7 〇3 9 N 1 1 9 2 o Experiment • C (please read the notes on the back side first (This page is written) This paper scale is applicable to the China Sleepy Family Standard (CNS) A 4 specifications (210 X 297 mm) -232 2139 (· i A6 B6 V. Invention description fe3〇) 67. 31, Η 7. Ο 8, Ν 11.71. Example 1 1 Ο 1 one (triple tributyl acetamide) a 3 — (3 — methyl tyramine tyramine and even a certain) a 5.7 — dirong very six argon xenon heterococoon 2 — ketone 1— (Third butylacetamide) —3— (3-aminophenylureido) —5,7-diphenylhexahydroazazepine—Class I, 69% yield, which is React with methanesulfonyl chloride in pyridine at room temperature, m ρ 185 -1 9 2 t: 〇 ^ -NMR (δ, CDaSOCDa): 1. 15 ((Please read the notes on the back before filling this page) — Installed · Printed the act Zaofeng t 9 H) 9 1 • 8 ― 2 • 0 (mt 3 H) 2 • 5 7 (mt 1 H) 9 2 • 9 4 (s 9 3 H) t 3 • 2 0 (m 9 1 Η) »3 • 5 〇 (ABQ 9 J Λ B: L 6, D n = 2 3 1 9 2 H) &gt; 5» 0 9 (d 9 J = 1 1 9 1 H) f 5 • 3 0 (d 9 J = 1 〇 »1 H) 9 6 • 6 a 7 ♦ 4 (mt 1 6 H) &gt; 9 • 1 1 (st 1 H) t 9 * 6 2 (sf 3 H) 〇1 3 C-NMR (δ> c D 3 S 0 CD 3) • 2 8 • 5 f 4 5 • 0 »4 7 • 0 9 4 9 • 9 $ 5 1 • 5 9 5 9 • 4 f 1 〇8 ♦ 3 9 1 2 6 • 8, 1 2 6 • 9 t 1 2 8 • 0 f 1 2 8 • 4 9 1 2 8 ♦ 5 t 1 2 8 • 6 * 1 2 8 • 7 t 1 2 9 • 3, 1 2 9 ♦ 4 »1 2 9 • 5» 1 2 9 • 6 t 1 3 9 • 3 t 1 4 1 • 4 negative 1 4 6 3 »1 5 3 • 6 9 1 6 7 • 3» 1 7 3 * 2 o IR (cm -1 9 KB r) • # 1 6 4 0 (width, C = = 0) 0 order _ This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm> _ 〇33 Β6 Printed by Employee Consumer Cooperative of Central Bureau of Standards of the Ministry of Economic Affairs 5. Description of Invention) FAB MS (96): 606 (parental +1, 47), 5 3 3 (6 4), 1 9 3 (1 0 0), 1 1 9 (6 3), 9 1 (59) 〇 Analysis and calculation of C32H33N5〇5S · 1 / 2H2〇: C 62.52, H 6. 5 6, N 11. 3 9, S 5. 22. Experiment: C 62. 12, Η 6. 8 0, Ν 11. 0 8, S 5.32. Fen Shi Example 111 1 1 (t-t dinghua acetamide) 1 3 1 (3 1 (N- 1m m Hua) phenylurea Hua) 5 • 7 Benhua—IU radon aza extraction 2 _ system white 1 — (Third butylacetamide) — 3 mono (3-aminophenyl m group) — 5 9 7 — diphenyl-L-. Hydrogen krypton leather 2-ketone> 4 5% yield 9 which Yi and methyl isocyanate reacted in refluxing tetrahydrofuran 1 8 hr * m P 1 8 5 — 1 9 5 〇2 Η--Ν MR (δ, CDC) l 3) • 1 • 1 0 (single peak 9 9 Η) 9 1 • 9 — 2 • 2 (mt 3 Η) 9 2 • 5 (mt 1 Η) * 2 • 6 0 (b S, 3 Η) »3 • 0 4 and 3.8 (multiline 9 2 Η) »3 • 2 8 (m $ 1 Η) t 5 • 0-5 • 2 (wide multi-line 9 2 Η), 5 • 4 — 5 • 6 (wide multi-line t 2 Η) 9 6 • 8 — 7 • 4 (mt 1 5 Η) 9 7 .6 (b S »1 Η) &gt; 8 * 1 (bs 9 1 Η) 0 13 C-Ν Μ R (δ t CD c 1 3) 4 2 6. 6, 28.5, 46.0, 51.1, 126.9, (please read the notes on the back before filling in this page) Use China National Standards (CNS) Grade 4 specifications (210 X 297 mm) -234 A6 B6 2 II. V. Invention description Pan 32) 127.0, 128.4, 128.6, 1 2 8. 7, 128.8, 128.9, 129.0, 129.5 , 1 2 9. 6, Yu Shuo was not seen in this scan. IR (cm &quot; 2, KBr): 1640 (width, C = 0) Ο FAB MS (96): 585 (parent +1, 26), 512 (6 0), 193 (1 0 0), 115 (4 2), 9 1 (58) 〇Analysis calculation C 33Η μΝ 6〇4 ♦ Η 2〇: C 6 5.76

, Η 7. 0 2, Ν 13. 94. Experiment: C 65.94, Η 6.74, Ν 13.58. Fen Shi Example 112 Ν — (1-methylcyclohexyl) 2 — “3-bromo-2—hydrogen 5— (fumou) one 2. 3. 4. 5-Siqiyi 1Η — Μ) Rongyou Gas mixture cover 1 1 1 1 ethyl acetamide according to Example 1 using N-(1-methylcyclohexyl) iodoacetamide to 3-Mo 2-gas 5-(phenyl)-2, 3, 4, 5 — tetrahydro-1H— (1) benzoazepine-based, mp 16 4 — 1 6 8 t 〇'H-NMR (δ, CDCI3): 1.35 (s, 9 Η), 1.46 (s, 3 Η), 1. 2-1.5 and 1.9-2. 1 (m, 10 Η), 2. 62 and 2.79 (2 multiplex lines of diastereomers, 1 Η), 2. 92 (m, 1Η (Please read the precautions on the back before filling in this page) -Installation. Order _ — ^ _ Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. The paper size is compliant with China National Standard (CNS) A4 specifications ( 210 X 297 mm> -235 A6

2139k! _E 5. Description of the invention &amp; 33)) &gt; 4 • 2 —— 4 • 7 (m 9 4 H) 9 6 • 0 and 6 • 1 1 (DO early peak t 1 H) &gt; 6 • 6 — 7 • 4 (m * 9 H) 〇13 c — NMR (δ &gt; CDC 1 3) 12 1. 9, 2 2 • 0 9 2 5 • 5 f 2 6 • 4 1 3 6 • 3 t 3 6 • 9 9 4 3 • 0 t 4 3 • 1 9 4 4 • 1 t 4 4 • 8 9 4 7 • 1 9 5 3 • 7 * 5 4 • 8 t 5 5 • 1 $ 5 6 • 5 9 1 2 3 • 2 t 1 2 7 • 5 t 1 2 7 • 6 »1 2 7 ♦ 7 t 1 2 7 • 8» 1 2 8 • 0 t 1 2 8 • 1 f 1 2 8 • 7 1 2 8 • 8 f 1 2 9 • 0 t 1 3 7 • 5 f 1 3 7 • 7 t 1 3 9 ♦ 0 t 1 4 0 • 7 t 1 4 1 ♦ 1, 1 6 7 • 1 »1 6 8 • 2 f 1 6 8 # 7 o IR (C m -i 9 KB Γ) • 1 6 6 0 wide (C = 0) 〇MS (%) • 4 6 8/4 7 0 (parent B r 7 9 / B r 8 J t 1/1) t 2 7 6 (5 〇) f 2 5 0 (5 1) t 1 6 5 (4 0) f 9 7 (3 8) »5 5 (1 0 0) 〇 (Please read first Remarks on the back and then write this page)-Pack. Order. 'N— (l—methylcyclohexyl) 2 — [3—II 氤 一 2 — —5 — (Juki) 1. 2. 4. 4. 5 — Siqiyi 1H — (1) The Ronghe M Misha-1 printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs -1, 1 base Ίethyl acetamide 1 Preparation, 4 1% yield oil. iH-NMR (5, CDC13): 1.29 (s, 9 Η), 1.4 3 (s, 3 Η), 1.1-1.6 and 1.8-2.0 (m, 1 0 Η), 2.7 .6 (m, 1 Η), 2 • 9 2 (m ， 1 Η) »3 • 0 9 (A Β qf tJ Λ = This paper scale applies the Chinese National Standard (CNS) A4 specifications ( 210 X 297 mm) -236 A6 B6 Printed by the Ministry of Economic Affairs, Central Standard Shell Industry Consumer Cooperative V. Invention description 34) 1 5 »dn = 3 1 7 t 2 H) &gt; 3 • 9 7 (m» 1 H) f 4 • 2 0 (m »1 H) &gt; 6 • 1 8 (bst 1 H) t 6 • 9 — 7 • 5 (m 9 9 H) o 1 3 C — NMR (δ t CD c 1 3) &lt;: 2] L. 8, 2 2 ♦ 0 * 2 5 «5 &gt; 2 6 • 4 &gt; 3 5 • 7» 3 5 • 8 &gt; 3 6 • 0 9 3 6 • 1 t 3 6 • 3 »3 6 • 9» 3 7 • 0 $ 4 3 • 7 &gt; 5 3 • 4 t 5 4 • 7 9 5 8 • 4 »1 2 5 • 5» 1 2 5 • 6, 1 2 5 ♦ 7 1 2 5 • 8 * 1 2 5 • 9 »1 2 6 • 0 &gt; 1 2 6 • 2 9 1 2 6 • 5 t 1 2 6 * 6 f 1 2 6 • 7 9 1 2 7 * 3 9 1 2 7 • 5 $ 1 2 7 • 6 f 1 2 7 • 7 f 1 2 8 * 0 t 1 2 8 • 5 * 1 2 8 • 7 t 1 2 9 • 2 9 1 2 9 3 t 1 3 0 • 3 9 1 3 0 • 4 9 1 3 7 9 f 1 4 1 • 0 9 1 4 1 • 1, 1 6 8 • 0 • 1 7 0 • 0 0 IR (C m -i &gt; KB r) • • 2 1 0 0 (N 3) and 1 6 7 5 width (C = 0) o FABMS (%) • 4 3 2 (parent + 1 t 3 2) t 4 0 6 (7 0) 9 3 1 9 (1 0 0) t 2 9 3 (9 2) 9 1 9 4 (9 0) t 9 1 (9 2) 〇Η RM s Calculate C 2 5 H 2 9 N 5 0 2 • 4 3 1 • 2 3 1 5 〇Experiment • • 4 3 1 • 2 3 1 3 5 o (please read the precautions on the back before filling in this page). Pack · Order-N — (1 —Methyl-hexyl) 2 — Γ3 —Aminyl 2 —Argon 5-(Benyl) —3 * 4 t 5 —Tetra Gas—1H-(1) This paper scale is applicable to the Chinese National Standard (CNS ) A 4 specifications (210 X 297 mm) _ 〇37 A6 B6 V. Description of the invention 035) Zhuzhuang xenon hybrid _ 1-a Ίethethoxamine prepared according to Example 1, a white foam in 69% yield. JH-NMR (5, CDC13): 1.26 (s, printed by the Employees Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 9 Η) $ 1 • 3 9 (s 3 H) »1 • 0 1 1 7 and 1 • 8 1 2 • 0 (m 9 1 0 H) &gt; 2 • 2 2 (bst 2 H 9 Ν Η. _2) 9 2 • 5 (m $ 1 H) t 2 • 7 8 (mf 1 H) &gt; 3 • 0 8 (AB? 9 J Λ B: two 15, dn = 3 0 5, 2 Η) t 3 • 4 8 (mf 1 H) t 4 • 1 0 (m »1 H)» 6 • 1 0 (bs » 1 H) t 6 • 9-7 • 4 (m »9 Η) ο 13 C-NMR (δ t CDC 1 3): 2] L. 9, 2 5 • 5 $ 2 6 • 4 9 3 1 • 5 See 3 6 • 2 9 3 6 * 8 9 3 9 • 7 f 4 4 • 5 f 5 0 • 7 1 5 3 • 4 t 5 4 • 4 $ 1 2 5 • 3 9 1 2 5 • 4 9 1 2 5 • 5, 1 2 6 • 2 t 1 2 7 • 2 9 1 2 8 • 3 9 1 2 8 • 5, 1 2 8 • 8 »1 3 0 • 2, 1 3 8 • 7 t 1 4 1 • 6 9 1 4 1 • 8 &gt; 1 6 8 • 3 &gt; 1 7 5 • 1 〇IR (cm -1 »KB Γ) • • 1 6 6 0 width (c — 0) o FABM s (96) • 4 0 6 (Parent + 1 t 8 4) t 2 9 3 (1 0 0) t 2 3 7 (3 8) 9 1 9 4 (4 3) o Η RM s Calculate C 2 5 H 3 1 N 3 0 2 • »4 0 5 • 2 4 0 9 o Experiment • 4 〇5 • 2 3 8 0 7 o Ν (1 Lihuahuan P, Hua) 2 〔3 (3 (3 (please read the precautions on the back before writing this page) i install-order-| Izumi _ this paper The scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -238

Fifth, the invention description gold 36) Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs, Benhua) Adena) 1 2 ― Oxygen (Benza) — pf 3 4 5 Tetrahydrogen 1 Η (1) Benzot Cui 1 Hua 1 Acetylamide according to Example 1 Whitening * Ν ― (1 monomethylcyclohexyl) 2 — C 3 — Amino one 2 ― Gas ― 5 — (phenyl) ― 2 t 3 $ 4 t 5 ― Tetrahydro-1 Η ― (1) benzoazepine ― 1 ― yl) Acetamide 9 m P 1 3 0 ― 1 4 0 V »9 4% yield Ο 2 Η--NMR (δ, CDC ] [3) * • 1 • 1 6 (t, J = 8 9 3 Η) 9 1 • 2 8 (S 9 9 Η) »1 • 3 7 (s 9 3 Η) &gt; 1 • 2 a 1 • 5 (mt 6 Η) 9 1 «8 one 2 • 0 (mt 4 Η) 2 • 5 4 (qf J = 8 9 2 H)» 2 • 9 and 3 • 1 (m ref 2 Η) »3» 2 4 (AB 9 9 J Λ B: =) L 6 9 d η 2 9 7 t 2 Η) t 4 • 2 2 (dt J = 8 t 1 H), 4 • 6 6 (m 9 1 H) 5 0 9 0 (b S f 1 H), 6 • 5-7 • 4 (mf 1 3 H), 7 * 7 1 (bs &gt; 1 H) Ο i 3 C ― N Μ R (δ 9 CDC 1 3): 15.6, 2 1 • 9, 2 2 • 0 9 2 5 • 4 9 2 6 • 1 $ 2 8 * 9 f 3 6 φ 4 9 3 6 • 6 9 3 7 • 3 9 4 4 • 4 $ 5 0 • 1 t 5 3 • 8 f 5 4 • 0 9 1 1 7 • 2 t 1 1 9 * 6 t 1 1 9 • 7 »1 2 2 • 5 &gt; 1 2 4» 9 1 2 5 ♦ 0 »1 2 6 • 3 f 1 2 6 • 4 $ 1 2 7 • 8» 1 2 7 • 9 »1 2 8 • 4 9 1 2 8 • 8 t 1 2 8 • 9 t 1 2 9 • 0 »1 3 0 • 7 &gt; 1 3 0 • 8 f 1 3 8 • 3 t 1 3 9 • 1 t 1 4 1 • 2 &gt; 1 4 1 • 8 $ 1 4 5 • 3 t 1 5 5 • 4 »(Please read the precautions on the back before filling in this page) — Binding · Order · • Elephant-This paper standard is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -239 2139Gj A6 B6

V. Description of invention fe37) Printed by Beigong Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs 1 6 7 • 7 »1 7 3 ♦ 0 〇IR (cm -1 I κ Β r) • 1 6 5 0 寛 (C = 0) o FA Β Μ S (%): 5 5 3 (parent + 1 »3 2) t 4 4 0 (6 8) 9 2 9 3 (8 4) t 2 2 0 (8 2) t 1 9 4 ( 1 0 0) 9 9 1 (5 6) 〇Analysis calculation C 3 4 Η 4 0 N 4 0 3 ♦ 1/4 Η 2 0 *: C 7 3 • 2 9 t Η 7 • 3 3, Ν 1 0 • 0 5 〇Experiment • c 7 3 • 3 0 9 Η 7 • 1 5, Ν 1 0 • 2 5 〇jing Example 1 1 3 N (Jiahua ring body extract) 2 — r 3 (3 (3 gas benzene Hua) m Hua) Oxygen-5 (Benzhua) • 3 «4 • 5 Tetragen 1 Η (1) Benzodiazepine 1 Hua] r 丨 Acid acid according to Example 1 0 7 Whitening» N-(1 (Methylcyclohexyl) 2 -c 3-Amino-2-Gas-5-(phenyl)-2 t 3 t 4 t 5-Tetrahydro-1 Η-(1) Benzo-triazine 1- Group] Acetamide Acetate fm P 2 1 5 1 2 2 0 V t 8 4% yield Ο 1 Η--NMR (δ, CDC 1 ί 3) • ♦ 1 • 2 8 (s 9 9 Η), 1 • 3 6 (s 9 3 Η) f 1 «2-1 • 5 (m» 6 Η) 1 • 8 — 2 • 0 (mf 4 Η) t 2 • 9 — 3 • 0 (m $ 2 Η) &gt; 3 • 3 3 (A Β Q t J Λ Β = 1 -6, d η = 2 8 4 &gt; 2 Η) »4 * 2 6 (d 9 J = 7» 1 Η) f 4 • 6 3 (m »1 Η) 9 5. 7 9 (bs» 1 Η) t 6 6 a 7 6 ( mf 1 3 Η) f 7 9 9 (bs »1 H (please read the precautions on the back and then $ this page) This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -240 i A6 B6 5. Description of the invention &amp; 38) 〇13 C-NMR (δ f CDC 1 3) «4: 22.0, 2 2 • 1 9 2 5 • 4 9 2 5 ♦ 9 9 3 6 • 4» 3 6 • 7 »3 6 • 9 9 4 4 • 5 9 5 3 • 4 9 5 4 • 1 t 1 1 7 • 1 9 1 1 9 • 1 t 1 2 2 • 2» 1 2 4 • 4 »1 2 4 • 5 t 1 2 6 • 3 t 1 2 6 • 5 f 1 2 6 • 6 »1 2 7 • 8 t 1 2 8 • 4 t 1 2 9 • 1 t 1 2 9 * 6 f 1 3 0 • 8 f 1 3 4 • 3 $ 1 3 8 • 2 t 1 4 0 • 7 »1 4 1 • 1 t 1 4 1 • 7 &gt; 1 5 5 • 1 i 1 6 7 • 4 »1 7 3 • 2 〇IR (cm -1 * KB r): 1 6 5 0 width (C 0) o FABM s (%) ♦ • 5 5 9/5 6 1 (parent + 1 &gt; C 1 3 5 / C 1 3 7 2 1/8) 9 4 4 6 (6 9), 2 9 3 (5 5) 9 2 3 7 (5 8) t 2 2 0 (9 2) »1 9 4 (1 0 0) t 9 7 (8 0) O Analytical calculation C 3 2 H 3 5 N 4 0 3 C 1 • C 6 8 * 7 4 9 H 6 • 3 1 t N 1 0 • 0 2 0 experiment • • C 6 8 »4 0 t H 6 1 9 9 N 9 8 2 0 (please read the precautions on the back before filling this page) Printed by the Bureau of Standards, S Industry and Consumer Cooperatives 114 N-(1-a certain cyclohexyl group) 2-"3-(3-(3-methylbenzyl) gland group)-2-Qiyi 5-(benzyl ) ~ 2. 3. 4. 5_ 四 气 一 1H_ (1) Juxenon hetero-cap 1_yl Ίacetamide acetate was prepared according to Example 107, N— (1-methylcyclohexyl) 2 — [3 —Amino one 2 —Gas one 5 — (phenyl) —2,3,4,5—Four paper scales are applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -241-A6 Ministry of Economic Affairs Central Engineering Bureau Printed by the consumer cooperative V. Description of the invention 39) Hydrogen 1 Η 1 (1) benzodiazepine 1 1 yl] Acetamide Acetate 9 m P 2 2 0 ― 2 2 5 t: »8 5% Yield oi Η--NMR (δ i, CDC] ί 3) • 1 • 2 8 (S 9 9 Η) t 1 • 3 8 (st 3 H) t 1 • 2-1 • 5 (m 9 6 Η) $ 1 • 8-2 • 0 (m »4 H) $ 2 • 2 3 (st 3 Η)% 2 • 8 (mf 1 H) $ 3 • 0 6 (mt 1 H) i 3 • 2 2 (AB 4 t J ί Λ θ = 1 6, dn = 2 9 7, 2 H) t 4 • 2 3 (dt J = 8 minus 1 H) f 4 • 6 5 (mt 1 H), 5 • 9 〇 (bst 1 H) t 6 «5 ― 7 t 4 (mt 1 3 Η) 7 • 6 8 (bs 1 H) o 1 3 C ― NMR (δ t CDC 1 3): 2] L. 5, 2 1 • 9 f 2 2 • 0 »2 5 • 5 t 2 6» 1 f 3 6 • 4 »3 7 • 2 t 4 4 • 4 food 5 0 • 1 t 5 3 • 8, 5 3 • 9» 1 1 6 • 9 t 1 1 7 • 0 »1 2 0 • 6 t 1 2 3 • 7 t 1 2 4 • 9 &gt; 1 2 6« 3 »1 2 6 * 5 y 1 2 7 • 8 1 2 8 • 3 &gt; 1 2 8 • 5 t 1 2 8 • 7 t 1 2 9 • 0 9 1 2 9 • 1 f 1 3 0 • 7 t 1 3 0 • 8 • 1 3 8 • 3 »1 3 8 • 8 t 1 3 9 * 0 f 1 4 1 • 2 t 1 4 1 • 8 $ 1 5 5 • 3 t 1 6 7 • 6 9 1 7 2 • 9 0 IR (cm -1> KB r) • • 1 6 5 0 width (C = 0) 〇FABM s (96) • • 5 3 9 (parent + 1 t 6 0) f 4 2 6 (8 2) 9 2 9 3 (9 2) t 2 2 0 (9 4) »1 9 4 (1 0 0) 9 1 1 9 (7 3) 9 7 (7 1) »9 1 (99) 〇 (Please read the precautions on the back before filling in this page) 1 '.—Packing. Order. R This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm)- 242 Central Standard of the Ministry of Economic Affairs, W, Consumer Cooperation, Thorium Printing A6 B6 V. Description of invention fe40) Endeavour Example 115 2 — (Cui P. 某) 一 2 —Rongmou ^ Alcohol is equipped with a condenser and 500 mi of N2 inlet? In a round-bottom flask, add 15g (68.8 · · 〇1) 〇 (-phenyl truncated hexyl acetic acid, 110 anhydrous tetrahydrofuran, and 137mj? (275mm〇l) 2M borane monomethyl sulfide in tetrahydrofuran Solution. This liquid was refluxed for 60 hours, cooled and evaporated. The residue was carefully ingested in 200mi ethanol, treated with 2g sodium carbonate, and refluxed for 3hr. The reaction was cooled, evaporated, taken up in ethyl acetate / water, separated, and the aqueous phase was extracted with fresh ethyl acetate. The organic layers were combined, washed with brine, dried over sodium sulfate, and evaporated to an oil, which solidified when left standing. The yield is 12.27g (87%). 2H-NMR (δ, CDC13): 0.7-1.9 (m, 1H), 2.54 (m, 1H), 3. 7-3. 9 (m, 2H), 7.1-7.3 (m, 5H). 2 -(顼 H 某) —2 —Rongmou ethanol ethanol methyl androst ester 125mi? Round bottom flask was added 12. 27g (6 0. 15 «ηιη〇1) 2 — (cyclohexyl) a 2-phenylethanol and 30 mi? Anhydrous pyridine. The reaction was cooled to 〇10, and 13.78 (7 2. 18 mmo1) tosylate was added. Reaction at Ot: place for 14hr, pour into water, and extract with ether. The ether layer was washed with 3 parts of IN hydrochloric acid, 3 parts of a saturated aqueous solution of sodium hydrogenate, 2 parts of water, and brine, dried over sodium sulfate, and evaporated. The residue is slurried in ethanol and collected by filtration to produce white (please read the precautions on the back and then f ^ page).-Packing. _ This paper size is applicable to the a® family standard (CNS) A 4 specifications (210 X 297 Mm) -243 A6 B6 printed by the 8th Industrial and Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 5. Description of invention) Solid, mp 95-100¾. 13. lg (61¾) 〇'H-NMR (δ, CDCIJ: 0.6-1.7 ( m, 1 1 Η), 2.40 (s, 3 Η), 2.64 (m, 1 Η), 4.1-4.3 (m, 2 Η) · 6. 9-7.5 (m, 5 Η) 0 IR (cm, KBr): 2940 (CH) and 1 6 0 0 (C = C) 〇MS (%): 186 (100, no tosicacid parents), 104 (95), 91 (70 ). Analysis and calculation of ChH26〇3S: C 70 · 35, Η 7. 31. Experiment: C 70. 32, Η 7. 3 3 〇2 — (ring R certain) -2- phenyl -1- _ Yiyuan. . In a 25〇mJ2 national bottom flask equipped with a condenser and N2 inlet, add 13.9g (39.4mm〇l) 2- (cyclohexyl) -2-phenylethanol tosylate, 80mi acetone and 6.49g. (43.3 mmol) sodium iodide. The reaction was refluxed for 36 hr, cooled, and evaporated. The residue was taken up in ethyl acetate, washed with water and aqueous sodium bisulfite solution, and washed with sodium sulfate Dry and evaporate to an oil, 12.11g (98%), directly used in the next step. 'H-NMR (δ, CDCla): 0.7-1.9 (m, 1 1H), 2. 60 (m, 1H) , 3. 4 and 3. 6 (m, 2H), 7.0-7.3 (m, 5H) 〇 (please read the note $ item first and then write this page) — Pack. Order. This paper size is applicable to Chinese national standards (CNS) A 4 specifications (210 X 297 mm) -244 Α6 _Β6_ V. Description of invention fe42) Diethyl (2 — 瑗 hexyl) 1-2 — Rong Moumou) Propylene dihydroxide ester equipped with a condenser and N2 inlet To the 50〇1115 round-bottom flask, 3.05 g (77 · 1 «» 〇1) of hydrogenated sodium was added, which was washed with hexane and sucked off hexane, and 100 mi of anhydrous tetrahydrofuran. A solution of 12.34 g (77.1 ·· 〇1) diethyl malonate in 50m of anhydrous tetrahydrofuran was added dropwise to the stirred suspension over 30 minutes. Once the gas evolution was stopped, a solution of 12. llg (38.57 mmol) 2 — (hexyl) -2-phenyl-1-iodoacetate in 40 anhydrous tetrahydrofuran was added, and the reaction was refluxed for 3 days. The reaction was concentrated, poured into 1N hydrochloric acid, and extracted twice with ethyl acetate. The combined organic layer was washed with water, 3 parts, aqueous sodium bisulfite solution, and brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel, using hexane / ethyl acetate as the eluent, to produce an oil, 12. 5 3 g (87%) 〇 &quot; H-NMR (5, CDCla): 0.6-2.0 ((please (Pay attention to the item Ϋ before writing this page). 丨 Install-H 2 2 1 ± 7 Η 3 o 2

H 3 9 7-J Η 1X 9m / l \ 4 2 • 2 H 1X fm / lx 2 3 • 2 5 9 • 2 4 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs)) 1 o, 6 H H3) 3 5 2. 2 5 1,, .9,, c 5 7 8 6 mmD.. 2 1 ((c 6 9 1, 8 2, 2 4, 4 9.5 ,, 3..7 (43. 9 3-R . · 6 6, 9 M 6 3 2 1) .N 241 »H 6 I,,,, 6 1 * c 1 o 2 · 3 2 f \ J 1 ··· * · ^ ι OH 4 2 14 121 006- 1 5 1X 4 9 ♦ 3 2 0 • · &gt; 1 15 3 6.,, 8 13 2, · 1 The paper size is applicable to China National Standard (CNS) Grade 4 (210 X 297 mm) -245 Ministry of Economic Affairs Printed by the Central Bureau of Standards, 8 Industrial and Consumer Cooperatives A6 B6 V. Description of invention ^ 43) IR (cm-2, KBr): 1 7 3 8 (C = 〇) 〇MS (96): 346 (parent, 12), 160 (100), 114 (60), 28 (59) ^^ 1 ruler 1 ^ 13 calculation (: 221 ^ 3.〇4: 346.2 1 36. Experiment: 346.213838. 3 monocyclohexyl-3-phenylbutane The 250mi bottom flask equipped with a condenser and N2 inlet was filled with 12.53g (36. 2 mmol) diethyl-2- (chenhexyl) -2-phenethyl) malonate, 80mi acid, And 25χηί 6Ν hydrochloric acid. The reaction was refluxed for 20hr, cooled, poured into water, ethyl acetate Ester extraction. The organic phase was washed with water and brine, dried with sodium sulfate and evaporated. The trace water was evaporated from heptane to produce oil, 9.78s (99% unprocessed yield). ^ -NMR (δ, C Ό C \ 3 ): 0.8, 2 3 (m, 16H), 7.0-7. 3 (m, 5H) 〇i3C-NMR (δ, CDCIj): 26. 5 27. 7, 31. 2, 31. 3, 32 . 6, 4s 2 ^ 51. 6, 43. 2, 51. 6, 1 2 6. a &gt; 128.3, 128.5, 143.3, 8〇IR (cm_i, KBr): 1720 (Cs ^ q) MS (96) : 246 (parent, 13), 173 (45), 163 (52), 117 (78), i04 (100), 91 (79), 5 (48) 〇HRMS calculation ChH22〇2 : 246. L6l4. (Please read the precautions on the back before filling in this page)-Pack. The size of the paper is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -246 A6 B6 V. Invention description Pan 44) ( Please read the precautions on the back before writing this page) Test: 246. 15968. The rest of the steps were carried out as in the similar compound in Example 2: 4-A single one 1. 2. 3. 4-Four dianthus 1-1 — An oil with a yield of 74% was prepared. i Η--Ν Μ R (δ, CDC] i 3) • • 1 • 9-2 • 1 (m 9 5 Η) t 1 • 4 — 1 • 8 (mt 6 H) t 2 • 0 — 2 ♦ 2 (m 9 2 H) 9 2 • 4 one 2 • 7 (m 9 3 H) 9 7 * 0 — 7 9 3 (m 9 3 H) 9 7 • 8 8 (m 9 1 H) O 1 3 C — Ν MR (δ 9 CD c 1 3): 2 4. 3, 2 6 * 3 9 2 6 • 5 t 3 0 • 5 1 3 5 • 0 9 3 9 ♦ 9, 4 4 • 0 f 1 2 6 • 6 t 1 2 7 • 4 9 1 2 9 • 2, 1 3 2 • 3 t 1 3 2 • 6 &gt; 1 4 7 • 3 9 1 9 8 • 6 0 IR (C m -1 1 KB Γ) • • 1 6 9 0 (C = 0) o Μ S (%) • 2 2 8 (parent »7) f 1 4 6 (1 0 0) t 5 5 (2 〇) o Η R Μ S meter &gt; rAr is calculated as C l 6 H 2 0 0 • 2 2 8 • 1 5 0 9 O Experiment: 228. 15016. Printed by the 8th Industrial Consumption Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 4. A three-pointed 1. 2. 3. 4—four gas H-1 1-one ketoxime. A solid, mp 12 ◦—123Ό, 71% yield. 2H-NMR (δ, CDCla): 0.8-1.7 (m, 1 1 Η), 1.8 8 (m, 1 Η), 2.1 2 (m, 1 Η), 2. 39 (m, 1 Η) ), 2. 79 (m, 2 Η) This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -247 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of invention t 7 • 0 7 • 3 (m 9 3 Η) * 7 • 7 7 (m »1 H) 〇13 c -N Μ R (δ t CDC 1 3): 20.5, 2 2 • 4 f 2 6 • 3 * 2 6 • 4 &gt; 3 1 • 0 3 2 • 0 9 3 8 • 8 »4 4 • 9 &gt; 1 2 4 • 6 9 1 2 6 • 6 t 1 2 8 • 5» 1 2 9 • 7 »1 2 9 • 9, 1 4 3 • 2 t 1 5 5 • 6 o IR (C m -i 9 κ Β Γ) • • 1 6 4 0 (C = 0) o Analysis calculation c 16 Η 2 1 Ν 0 C 7 8 • 9 7 »H 8 • 7 0 9 N 5 • 7 5 ο actual • C 7 8 • 8 3» H 8 • 7 4 * N 6 • 6 4 ο 5 ring p, Hua 2 • 3 • 4 «5 four gas 1 H (1) Benyou gas mixed leather 2-ketone prepared as a white solid» m Ρ 1 2 5 — 1 2 8 t t 8 0 96 yield 〇2 Η--NMR (δ, CDC] [3) • • 0 • 6-2 • 0 (m 9 1 2 Η) 9 2 • 2 — 2 • 4 (m 9 3 Η) 9 2 • 5 9 (m 9 1 Η) f 6 • 9 — 7 • 2 (m »4 Η) 9 8 • 8 0 (bst 1 Η) Ο 13 C — N Μ R (δ, CDC 1 3): 26. 3, 2 6 • 4 t 3 1 • 〇 »3 1 • 6 t 3 2 • 5» 3 2 • 7 9 3 8 7 f 4 5 8 &gt; 1 2 2 • 4 t 1 2 5 3 9 1 2 6. 9, 1 2 8. 6, 1 3 6. 3, 1 3 8. 2, (please read the precautions on page f before filling out this page) This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -248 A6 B6 Printed by Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Description Pan 46) 17 6. 1 〇IR (cm—, KBr): 1680 (C = 0) 〇MS { %): 243 (40, parent), 160 (10 0), 132 (3 2), 118 (3 7). Analysis and calculation of C26HmNO: C 78.97, H 8.70, N 5.75. Experiment: C 78. 77, Η 8. 7 1, N 5.66. 3 — Chunyi 5 — Yuanji 2. 3. 4. 5 — Siheyi ΙΗΙ (Ι) Moxenoxenium hood -2-one to obtain a white solid mp 104-107, 54% yield. iH-NMR (δ, CDCla): 0.6-2.0 (m, 1 1 Η), 2. 25 (m, 1 Η), 2.69 (m, 2H), 4.37 (dd, J = 7,11,1H ), 7. 0-7. 3 (m, 4 Η), 8. 90 (bs, 1 Η) Ο &quot; C-NMR (δ, CDC13): 26. 1, 2 6. 4, 30.3, 3 2. 3, 38. 0, 44. 2, 44.9, 48.0, 1 2 3. 1, 126.5, 126.9, 127.2, 1 3 5. 3, 137.3, 16 9. 6 〇Ν — 三 丁某 2 — "3-Chunyi 2-Hydrogen 5-瑗 R certain-2. 3. 4. 5-Siqiyi 1H-(1) zhu # 氤 杂 箪 一 1 (Please read the precautions on the f side before writing the book Page) 2-Installed and ordered. • X. This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -249 A6 B6 213301 V. Description of the invention (247) Monoyl] Acetamide Acetate A diastereoisomeric mixture was prepared, which was divided into lower polar isomers, mp 188-189.51C, 36% yield, and higher polar isomers, mp 190.5-192t :, 58% produced Lower polar isomers: iH-NMR (δ, CDCh): 0.4-2.0 ((Please read the notes on the back before writing this page) mt 1 1 H) t 1 • 3 6 (st 9 H ) 2 • 3 9 (m, 1 Η) »2 • 6 1 (mf 2 H) t 4 • 0 1 (AB 4 f JAB = 1 5 &gt; D n = 3 8 1 t 2 H) 1 4 • 5 9 (dd, J = 8 9 1 2 f 1 H) &gt; 6 • 2 5 (bst 1 H) 9 6 • 9-7 • 4 (mt 4 H) o 1 3 c-NMR (δ 1 CD c 1 3): 26.] L, 2 6 • 2 9 2 8 • 7 t 3 2 • 2 t 3 2 • 5 »4 0 • 1, 4 2 • 5 &gt; 4 7 • 4 f 5 0 ♦ 3 9 5 1 • 5 t 5 5 • 7, 1 2 4 • 7 t 1 2 7 • 5 &gt; 1 2 8 • 6 &gt; 1 3 1 • 4, 1 3 6 • 0 9 1 4 1 4 t 1 6 7 • 6 f 1 6 8 • 6 〇 ·-binding-order higher polar isomers: employees of the Central Bureau of Standards of the Ministry of Economic Affairs Printed by the consumer cooperative ^ -NMR (δ, CDC13): 0.6-1.9 (m, 1 1H), 1.31 (s, 9H), 2.06 (m, 1H), 2.65 (m, 2H ), 4. 26 (AB ,, J “= 15, Dn = 32, 2H), 4. 2 (m, 1 H)

, 6. 22 (bs, 1 H), 7. 1-7. 3 (m, 4 H) 〇 &quot; C-NMR (δ, CDCh): 26.0, this paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -250 2 i, &gt; 'jx &gt; S ~ A6 B6 V. Description of invention) 2 6 • 3 9 2 6 • 4, 2 6 • 4 »2 8 • 7 t 3 0 • 3, 3 2 • 0 t 3 7 • 7, 4 3 • 7 »4 5 • 4 9 4 8 • 1, 5 1 • 4 &gt; 5 4 ♦ 8, 1 2 3 • 6 9 1 2 6 • 1 t 1 2 7 • 5 9 1 2 7 .6 $ 1 2 7 • 7 Ref. 1 3 6 • 2 9 1 4 2 • 0 9 1 6 7 .1 t 1 6 8 • 4 〇N T T 荸?, 1 Γ 3 Sauce radon 2 Oxygen production, Hua __ 2 • 3 t 4 «5 —Four radon 1 ϋ (1) Benzene φ Cyanine leather 1 (Please read the precautions on the back before writing this page) 1 1 47% yield of a higher polarity diastereomer produced from a previous acetophenone amine, mp 136-139 ^ 0 &quot; H-NMR (δ, CDC13): 0.4-2.0 (Central Standard of the Ministry of Economic Affairs M1 1 Η printed by the Bureau ’s Consumer Cooperative »1 • 3 4 (s reference 9 H), 2. 2 2 (m, 1 Η) t 2 4 3 (m 9 2 H)» 3 • 8 4 (mf 1 H) 9 4 • 0 4 (AB 9 tj a B: L 5, D n = 2 9 1 9 2 H) »6 • 3 2 (bs $ 1 H) t 7 • 0 -7. 4 (m 4 Η) ο 1 3 c — NMR (δ &gt; CDC 1 3) ♦ • 2 6. 0, 2 6 • 1 &gt; 2 6 • 2 t 2 8 • 6 9 3 2 .2, 3 2 • 5, 3 6 • 6 t 4 0 • 2 9 4 7 • 7 »5 1 .5, 5 5 • 1, 5 8 • 4 f 1 2 4 • 6 9 1 2 7 • 4» 12 8 • 6 9 1 3 1 • 3 »1 3 6 • 4 1 4 0 disgrace 7 , 16 7 • 7 f 1 7 0 • 8 o The paper size is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -251 Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy 2: 1 A6 _B6_ V. Description of the invention (249) N — tributyl 2 — “3-amino 1 — 2 — gas — 5 — Jinji certain 2. 3. 4. 5 — Siqi 1H— (1) Zhu And xenon miscellaneous 1 _ some Ί ethene acetamide (please read the precautions on the back before writing this page) i installed _ order-made a solid, nip 105-1 15¾, fixed Λ yield. ^ -NMR (δ, CDC13): 0.4-1.7 (m 1 0 Η) $ 1 • 3 1 (s »9 H)» 1 • 9 8 (mt 1 Η) t 2. 1 8 (mf 1 H) t 2 • 3 9 (m »1 Η)» 2 • 6 2 (m $ 1 H) t 3 • 7 9 (mf 1 H) 9 4 • 0 8 (A Β &lt; 1 9 J Λ B = 1.5 , D n = 3 6 4, 2 H) &gt; 5 • 5 (b S f 2 H) 9 6 • 6 1 (b S »1 Η) t 7 • 0 1 7. 3 (mf 4 H) o 13 C -Ν Μ R (δ »CD c 1 3) 1 (: 25.9, 2 6 • 2, 2 8 * 7 9 3 2 Ref. 2 * 3 2 • 3 t 3 7 • 7 $ 3 9 • 9, 4 7 • 9 9 5 0 • 6 9 5 1 • 7 t 5 4 • 1 * 1 2 4 • 1, 1 2 7 • 3 9 1 2 8 • 5 1 3 1 • 6 f 1 3 6 • 6, 1 4 0 * 4 t 1 6 7 • 7 9 1 7 2 • 1 Ο Ν 丁丁华 2 ί 3 (3 (3 toluene hua) m Hua) 2-argon 5 ring cadaver, Hua 2 «3« 4 «5 Four 1 Η ί 1) Benzene radon mixed drought 1 Hua] 醹 醯 m prepared white solid skull tSU · 1 m P 2 2 5 — 2 2 8 V 9 6 7% yield ο J Η--Ν Μ R (δ , CDC] l 3) • • 0 • 5 4 (mf 1 Η) t 0. 8 — 1 • 8 (m »9 H)» 1 3 5 (S 9 This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) -252 Α6 Β6 Printed by the Employee Consumer Cooperative of the Ministry of Economic Affairs Central Standards Bureau , Description of invention hso) 9 Η) 9 2 • 0 — 2 • 2 (mt 2 Η), 2 »4 9 (m 9 1 Η) 9 2 • 6 4 (mt 1 Η) &gt; 4 • 1 7 (AB 9 9 JAB = 1 6 D η = 4 0 8 9 2 Η) I 4 • 5 2 (mt 1 Η) t 6 • 2 3 (d »J = 7 9 1 Η) t 6 • 2 8 (s 9 1 Η) 9 6 • 7 a 7 * 3 (m »8 Η) t 7 • 6 2 (s 9 1 Η) Ο 13 c — Ν Μ R (δ t CD c 1 3) 4«: 2 1 4, 2 6 • 1 f 2 6 • 2 f 2 6 • 3 f 2 8 • 7 »3 2 • 3 t 3 2 • 5 &gt; 3 7 • 6 f 4 0 • 4 9 4 8 • 2 f 5 0 • 6 t 5 1 • 8 9 5 4 • 0 9 1 1 6 • 8, 1 2 0 • 5 $ 1 2 3 • 4 &gt; 1 2 3 • 5 f 1 2 7 »3 9 1 2 8 • 4 t 1 2 8 • 5 &gt; 1 2 8 • 6 9 1 3 1 • 7 »1 3 6 ♦ 7 9 1 3 8 • 6, 1 3 9 • 0 I 1 4 0 ♦ 9 1 5 5 • 5% 1 6 7 • 5 t 1 7 4 ♦ 1 o Jing Shi 1 1 6 Ν 丁丁华 2 3 mmm (3 (3 atmosphere phenyl) urea) 2 oxygen 5 ring p, Hua 2 «3 • 4« 5 four gas 1 Η (1) benzo mm single 1 Hua Ί 酹 acetamide as in Example 1 1 5 White Ν-the first butyl 2-C 3 monoamine group-2-oxygen-5-cyclohexyl-2 9 3 f 4 f 5-tetrahydro-1 Η-( 1) Benzoazepine-1-yl) Acetamide Acetate gives white solid teng 9 m P 2 2 3 1 2 2 6 V 9 4 8% yield Ο iH-NMR (5, CDC13): 0 · 52 (m, (Please read the precautions on the back before writing this page) 丨 Install. Order.

T This paper scale is applicable to the Chinese National Standard (CNS) A 4 specifications (210 X 297 mm) -253 2 A6 B6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention Instructions (251) 1 Η), 0. 8 -1. 8 (m, 9 Η), 1. 37 (s, 9 Η), 1. 98 (m, 1 Η), 2. 13 (m, 1 Η), 2.48 (m, 1 H), 2.48 (m, 1H), 2.58 ( m, lH), 4. 23 (AB ,, J a B = 1 6, Dn = 40 8, 2H), 4.48 (m, lH), 6.28 (s, lH), 6. 39 (δ, J = 7 , 1 H), 6. 8-7. 3 (m, 7H), 7.55 (s, lH), 8.01 (s, lH) 0 i3C-NMR (δ, CDC13): 26, 1, 26.2, 28 . 7, 32. 3, 32. 5, 37. 2, 40. 3, 48. 2, 5 0. 7, 52. 1, 53. 6, 116. 9, 118.9, 119.0, 122. 1, 123.0, 127.4, 1 2 8. 6, 129.4, 131.8, 134.2, 136.6, 1 4 0.5, 140.7, 155.2, 167.4, 174.5. Fen Shi Example 117 N —Third Ding 2 — “3 — (3 — (3 —Bei Rongmou) Urea) One 2 —Argon 5 —Jingji 2.2.3 4. 5 —Tetra Argon A 1 Η — (1) Rong and Xenon heteroacid -1 1-yl Ί 酴 醮 amine as in Example 115 made from N- third butyl 2- [3-amino group 2-an oxygen-5-cyclohexyl 3, 4, 5 -tetrahydro-1H-(1) benzodiazepine-1 (yl)] acetamide acetate to obtain a white solid, mp 145-155¾. 61% yield. This paper scale applies the Chinese National Standard (CNS) A 4 Specifications (210 X 297 g; * ·)-〇54 (please read the precautions on the back before writing this page) A6 B6 5. Description of the invention (252) i Η-NMR (δ, CDC 1 3) • 0 • 4 8 (mt 1 Η) t 0 • 7 — 1 ♦ 7 (m 9 9 H) 1 • 3 0 (t »J = 7 • 5 * 1 H) 9 1 • 3 5 (s 9 9 H) t 1 • 9 1 2 • 1 (m »2 H), 2 • 4 7 (qt J = 7 • 5 $ 2 H) 9 2 • 6 2 (m 9 1 H) 9 4 • 1 6 (ABQ * J λ B ~ 1 6 t D n = 4 0 4 9 2 H) f 4 • 5 0 (m 9 1 H) 9 6 • 2 3 (dt J = 7 9 1 H) f 6 • 2 6 (s »1 H ) »6 • 7 a 7 • 3 (m 9 8 H), 7 • 6 3 (s 9 1 H) 〇13 C-NMR (δ t CDC 1 3) * 1:] L 5. 6, 2 6 »1 9 2 6 • 2 1 2 6 • 3 f 2 8 ♦ 7 2 8 • 9 f 3 2 • 3 9 3 2 • 5 »3 7 ♦ 7 t 4 0 • 4 t 4 8 ♦ 2 9 5 0 • 5 9 5 1 • 8 9 5 4 ♦ 1 9 1 1 7 ♦ 1 »1 1 9 • 4 t 1 1 9 • 5» 1 2 2 • 4 9 1 2 3 ♦ 4 9 1 2 3 «5 f 1 2 7 • 3 9 1 2 8 ♦ 5 f 1 2 8 ♦ 7 9 1 3 1 • 7 9 1 3 6 • 7 9 1 3 9 ♦ 0 * 1 4 0 • 9 9 1 4 5 • 1 $ 1 5 5 • 4 t 1 6 7 • 6 * 1 7 6 ♦ 0 〇 (Please read the note on the f-face first, and then write the copy I) -Installation_ Ordering-The Ministry of Economic Affairs Central Standard 曷 8 工 consumer cooperative printed sinus example 118 (4 one argon zhuji) one 4 one 镩 某 瑗 own _ Acetal according to J. Med-Chem., 1992, 35, 320-

324 was prepared as follows: A 1 L 2 flask equipped with 1 ^ 2 inlet was charged with 46.8 g (0.30 mol) cyclohexane-1,4-dione monoacetal acetal and 500 mi anhydrous tetrahydrofuran. The solution is cooled to a temperature of 78C. The paper size is in accordance with the Chinese National Standard (CNS) A4 specifications (210 X 297) -255 A6 B6 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. 5. Description of invention (253), 3 m i η was added dropwise 4-monofluorophenylmagnesium bromide in 2.0 mM solution of 2.0M in diethyl ether 150mi2 (0.30m〇l), the reaction was stirred for 10m i η and warmed to room temperature. The reaction was poured into ice / water, the layers were separated, and the aqueous phase was extracted with ether. The combined organic similarity sodium sulfate was dried and evaporated to an oil, which was crushed with ether to make a white, low-melting, solid tar, 24.3g (32¾) 0 2H-NMR (δ, CDC13): 1.6-1.8 (m, 4 Η ), 2. 05 (m, 4 H), 3. 95 (bs, 4H), 6.96 (m, 2H), 7.61 (m, 2 H) 0 i3C-NMR (δ, C Ό C \ 3): 30 . 7, 36. 7, 64. 2, 6 4.4, 7 2. 1, 108. 3, 1 1 4. 8, 1 1 5. 1, 1 2 6. 2, 1 2 6. 3, 1 4 4 〇MS (%): 234 (7, parental H2O), 123 (15), 99 (100), 86 (60) 〇4_ (4 argon Rongmou) a hexanone 5. Og (19.8 mm 〇l) 4-(4-gas phenyl)-4-hydroxyl hexan ketal acetal melt in 170mi dioxane with 5.0 g 10% sulfonated rake under 35p. Si hydrogen treatment 24hr, Then filter through Celite to remove the catalyst. The filtrate was treated with 100 m of Wenshui and 3.5 mL of concentrated hydrochloric acid, and mixed at room temperature for 24 hr. Evaporate the solution, adjust the pH to 8 with a saturated aqueous solution of sodium silicate, and use dichloromethane (please read the note on the f-face first and then the f-page) -installation. Order · This paper size is applicable to China National Standard (CNS) 4 Specifications (210 X 297 mm) -256 A6 B6 5. Description of the invention (254) (Please read the note on the back of the page before writing this page> Methane extraction. The organic layer is dried with sodium sulfate and evaporated. Residue Chromatography on silica and dichloromethane as eluent produced 2.9g (74%) of oil. ^ -NMR (5, CDC13): 1.83 (m, 2H), 2.12 (m , 2H), 2.42 (m, 4H), 2.9 6 (m, lH), 6.8-7.2 (m, 4H) 0 i3C-NMR (δ, CDC13): 34. 1, 35. 1, 41.3, 42.0 , 115.2, 115.5, 128.0, 1 2 8. 1, 140.4, 140.5, 159.9, 163.1. No mineral sulfonate was seen in this scan. IR (cm ·, CHC13): 1 7 0 5 (C = 0)

O MS (%): 192 (90), 135 (60), 122 (1 0 0), 109 (65), 57 (15) 〇 HRMS calculation C / 2Hi3FO: 1 92. 0947. Experiment: 192.0983. The rest of the synthesis was carried out in accordance with Example 60: Printed by the 8 Workers and Consumers Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs;? _One gas and one— (4 one argon Rongmou) P. _ produced oil, 9 3 stone yield. 'H-NMR (δ, CDC13): 1.9-3.7 (sequential multi-line, 7H), 4.67 and 5.34 (multi-line, 1H), 6.8-7.2 (m, 4H). This paper size is applicable to China National standard (cns) A4 specifications (210 x 297 mm) -257 Α6 _Β6_ V. Description of the invention (255) i3C-NMR (δ, CDCI3): 33. 4, 33. 9, 34. 3, 35. 9 , 40.4, 42. 8, 4 5. 5, 6 3. 2, 115.5, 1 1 5. 7, 128.0, 1 2 8. 1, 128.2, 128. 3, no carbonyl master was seen in this scan. MS (%): 226 (55, parent), 171 (85), 122 (1 0 0), 1 0 9 (9 5), 55 (4 5) (Please read the notes on the back before filling this page ) The Ministry of Economic Affairs, Central Bureau of Standards and Staff's consumer cooperation du-printed 2-phenyl-4- (4-monophenyl) cyclohexanone to produce oil with a 29% yield. ZH-NMR (δ, CDCla): 2.0-2.4 (m, 4H), 2.64 (m, 2H), 33.24 (m, lH), 3.79 (dd, J = 5,13, lH), 6.9 -7.4 (m, 9H) 0MS (96): 268 (100, parent), 224 (90), 135 (65), 122 (95), 109 (75), 9 1 (9 9) 2- Phenyl-4- (4-tetrabenzyl) cyclohexylidene-made light yellow solid, mp 192-1941C, 64% yield. 2H-NMR (δ, DMSO-de): 1.5-2. 2 (m, 4 Η), 3. 02 (m, 1 Η), 3.42 This paper scale is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm) _ 258 B6 V. Description of invention (256) Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (m 9 1 H) $ 3 • 6 6 (dd &gt; J = 4, 1 3 9 1 Η) t 7 * 0 — 7 • 3 (m $ 9 H) 〇l 3 C-NMR (δ t DMS 0-d 6): 24. 1, 3 2 # 7 »4 1 • 3 f 4 2 • 3 f 4 8 • 3 »1 1 4 • 9» 1 1 5 • 1 $ 1 2 6 • 0, 1 2 7 • 7 »1 2 8 • 5 9 1 2 8 • 6 t 1 2 8 • 9 t 1 4 1 • 5 t 1 4 2 • 0 t 1 5 8 • 7 t 1 5 9 • 1 2 $ 1 6 2 • 3 o 5 (4 gas Benhua) 7 Benhua gas first extraction s 1L to produce light yellow foam 9 5 3 96 Yield 〇2 Η--NMR (δ, CDC] L 3) «• 1 • 8-2 • 2 (mt 4 H) t 2 • 7 0 (m 9 2 H) f 2 • 9 3 (mf 1 Η) $ 4 • 5 8 (m 9 1 H) $ 5 ♦ 7 2 (bs 9 1 H) N ID 6 • 9 a 7 • 4 (m 9 9 H) 0 1 3 C — NMR (δ 9 CDC 1 3): 30.5, 3 6 • 2 negative 4 5 • 4 »4 6 • 2» 4 7 • 8 t 5 8 • 0 t 1 1 5 • 3 »1 1 5 • 6 t 1 1 5 • 7 t 1 1 6 • 0 f 1 2 5 ♦ 5 9 1 2 6 »3 9 1 2 7 * 6 9 1 2 8 • 0 t 1 2 8 • 4 &gt; 1 2 9 • 2 9 1 4 1 • 8, 1 4 1 • 9, 1 6 3 • 1 9 1 7 6 • 4 fo FABMS (%) • • 2 8 4 (1 0 0 9 parent + 1) 9 1 8 0 (3 7) 9 1 0 9 (1 0) f 9 1 (1 1) 〇 (Please read the precautions on the back before filling out this page) This paper size is applicable to China National Standard (CNS) A 4 specifications (210 X 297 mm ) ~ 259 A6 B6 Fifth, the description of the invention (257) 3-Zhang Yi 5-(4 Yiqi phenyl)-7-Zhu certain six argon argon leather-2-_ prepared foamy diastereomer mixture , 63% yield. 2H-NMR (δ, CDCli): 2.0-2.6 (m 9 4 Η) 9 3 • 1 2 (m 9 1 Η) t 4 ♦ 5 0 (m 9 1 Η), 4 • 8 6 and 4 • 9 8 (Multiple lines of diastereomers at 3 position 9 1 Η) 9 5 • 8 7 (b S 9 1 Η) Ν HJ, 6 • 9-7 • 4 (m 9 9 H) o 2 3 C — Ν Μ R (δ »CD c 1 3): 42.0, 4 2 • 6 9 4 4 • 1 f 4 6 • 2» 4 7 • 2 »5 0 • 3, 5 7 • 3% 5 7 • 6 9 5 9 • 1 t 1 1 5 • 5 9 1 1 5 • 8% 1 2 6 • 2 9 1 2 8 • 0 1 1 2 8 • 1 9 1 2 8 • 8 9 1 2 9 • 4 t 1 4 0 • 1 »1 4 1 • 0, 1 6 0 • 1 t 1 6 3 • 3 f 1 6 9 ♦ 6 OIR (C m -1 9 κ B Γ) • 1 6 7 0 (C = 0) 〇 Ν (Mr · — Second 1 Ding Hua) 2 Oxygen 3 Carrying (4 Benzene huahua) — 7 Monobenzine t-gas radon hybrid extraction 1 Wax amine to prepare foamy diastereoisomeric mixture, 73% Yield. (Please read the note $ item on the back before filling in this page)-丨 Install · Order-

T Printed by the R-Consumer Cooperative Society, Central Bureau of Standards, Ministry of Economic Affairs &quot; H-NMR (δ, CDC13): 1. 27 and 1. 29 (single peak of two diastereomers, 9H), 2. 0 -2 . 6 (m, 4H), 3. 1 (m, 1H), 3. 56 (m, 1H), 5. 02 (m, 1H), 5. 44 (m, 1H), 6.9-7.3 (m, 9H) 〇This paper scale is applicable to China National Standard (CNS) A4 specifications (210 X 297 mm) -260 Printed by the Central Bureau of Standards of the Ministry of Economic Affairs 3 Industrial and Consumer Cooperatives 213. 2 A6 _B6_ V. Description of invention (258) N -(第三 丁某) -2—Μ — · 3— # Xenon-5— (4-gas benzene) -7-phenyl-six-gas gas seal 1-1 made from ethylamine to produce foamy non- Enantiomeric mixture,% yield. JH-NMR (5, CDC13): 1. 28 and obtained foam,% yield. ^ H-NMR (δ, CDC13): 1.21 (s, (Please read f first The precautions on this page will be written on this page) 'Install · Order · r 1 • 3 6 (αο Early Peak 9 9 Η) »2 • 0 —— 2 • 3 (m $ 3 H) * 2 • 5 (m &gt; 1 Η), 3 • 1 0 (mt 1 Η) 9 3 • 5 1 and 3 • 7 9 (AB t QS &gt; JAB 1 5 * D n = 2 3 8 and 3 2 6 $ 2 Η) 4 • 1 and 4 • 5 2 (Multiple Line »1 Η) t 4 • 9 0 and 5 • 0 9 (multiple lines 9 1 Η) t 5 • 5 0 and 5 • 9 0 (DB early peak 9 1 Η) 9 6 • 9 — 7 • 5 (mt 9 Η) 0 13 C-N MR (δ t CD c 1 3) • _ 2 8. 7, 2 8 • 8 »3 7 * 1 9 3 7 • 6 &gt; 3 9 • 2 &gt; 4 0 • 5, 4 5 • 4 f 4 8 • 3 t 5 1 • 5 »5 2 • 1 t 6 0 • 9, 6 1 • 2 $ 6 2 • 0 t 1 1 5 • 5» 1 1 5 • 8 1 2 5 • 9 f 1 2 8 • 1 t 1 2 8 • 3 f 1 2 8 • 4 t 1 2 8 • 8 »1 2 9 • 0 ί 1 2 9 • 4 9 1 3 7 • 9 f 1 4 〇 • 1 t 1 6 7 • 5 t 1 7 0 • 7 $ 1 7 2 • 2 〇N (--- butyl) 2 gas 3 amino group 5 (4-argon Moshen) 7 MM Hexaargon xenon hybrid _ 1 _ certain B The standard of this paper is in accordance with Chinese National Standard (CNS) A4 specifications (210 X 297 mm). -261 Printed by the Central Bureau of Standards of the Ministry of Economic Affairs, W Industrial and Consumer Cooperatives $ A6 B6 V. Description of Invention (259) 9H), 2. 0 -2. 3 (m, 3H), 2. 70 (m, 1H), 3. 30 (multiline, 3H), 3.73 (AB «» J ab = 1 Ύ, D n = 1 7 8, 2 H), 4. 80 (d, J = 1 1, 1 H), 5. 23 (d, J = 1 1, 1 H), 6.9-7.4 (m, 9H) 〇N— (third butyl) —2—gas—3— (3—Tian Rongmou carp—one 5 — (4 氱 phenyl) — 7 — stupid hexa-gas mixed leather -11-brewed amine to produce an amorphous solid, 62% yield. ^ H-NMR (5, CDC13, TFA): 1.20 (s, 9 H), 1.9 — 2.4 (m, 4 H) · 2. 33 (s, 3 H), 3. 26 (m, 1H) , 3. 8-4. 〇 (m, 3H), 5. 23 (m, 1H), 5. 37 (m, 1H), 6. 9-7.5 (m, 15H) 〇 Fen Shi Example 1 1 9 M- = ~~ (Jl tributyl) _ one 2 -chloro-3-(3-gas turbid Xiping) _ one 5 two __ (4-fluorophenyl) __ one 7-Zhu Ji one Hexaargon-xenon heteropyrene—1 _ prepared according to Example 118 from 1 \ 1— (third butyl) _2—gas—3 ~ amino-5— (4-fluorophenyl) —7-phenylhexahydrogen 5% 貦 皮基 acetamide, to obtain amorphous solid hydrazine, 54.5% yield. ^ -NMR (δ, CDC13, TFA): 1.2 〇 ---------------- Μ (please read 4? ^ The precautions before filling in the form page) bound book The paper scale is applicable to the China Sleepy Family Standard (CNS) A4 specification (210 X 297 g; t) -262 A6 B6 5. Description of the invention (260) (s, 9 Η), 2. 00 (m, 1 Η), 2 . 2-2. 5 (m, 3 Η), 3. 29 (m, 1 Η), 3. 86 (m, 1H), 3. 91 (AB ,, J AB = 1 6, Dn = 42, 2 H), 5 · 2 5 (d, J = 1 1, 1 H), 5. 41 (d, J = 1 1, 1 H), 6. 9-7.4 (m, 1 5 H) O Example 1 2 0 N — (the third Dingmou) one 2 —S— 3 — (3 —methyl argon and a certain urea) a 5 one (4 one argon mining a certain 7 one Zhu a certain six 氤 氤 heteroyl -1 1 基 乙Acylamine ----------------- 1, ------ Installed ------ ordered (please read the precautions on the back before filling in this page) Ministry of Economic Affairs Central Bureau of Standards®: Printed by the Industrial and Consumer Cooperatives according to Example 118, made from N — (third butyl) — 2-gas — 3-amino — 5 — (4-gas phenyl) — 7-phenyl monohexahydrogen Miscellaneous leather 1-1 acetylacetamide obtained an amorphous solid with a 55% yield oi Η -NMR (δ, CDC: 1 3 f T FA): 1. 1 9 (S &gt; 9 Η), 1. 9 7 (m »1 H)» 2 .2 — 2. 5 (m 9 3 Η), 3.2. 9 (mt 1 H) » 3 .8 2 (sf 3 Η) f 3 .8 3 (m »1 H) f 3 • 9 2 (AB? $ JAB = 1 7, D η = 5 1» 2 H) &gt; 5 • 2 3 ( d, J = 1 1 &gt; 1 Η), 5.3 8 (d »J 1 1» 1 H) »6 • 7-7.4 (m, 1 5 H) 0 This paper size is applicable to Chinese national standards ( CNS) A 4 specifications (210 X 297 mm) -263 ............... Qing RI1… 1,

Claims (5)

9 3 21 Announcement. Year 〇 Application for a patent model garden Annex II A: Patent Application No. 81110 0 4 4 Chinese application for a patent model garden amendment Amendment in May 1982 1. A compound of the formula Or rt>: where Y1 and Y2 are each selected from phenyl, benzyl, (C3-Cs) linear or branched-chain alkyl, (C5-Ce) cycloalkyl and (c5-c8) cycloalkyl one (Ci-Cs) alkyl group, wherein the phenyl group can be optionally substituted by-or two selected from halo, (Ci-C6) alkyl, (Ci-Ce) alkoxy and trifluoromethyl Substituted by a group; Z1 and Z2 are each selected from halogen-containing, (Ci-Cs) alkyl, (Ci-C6) alkoxy, (Ci-Ce) sulfanyl, trifluoromethyl, (---- ----------- Μ -------- installed ------ ir ---- ^ line (please read the precautions on the back before writing this page) The paper size printed by the Central Standards Bureau of the Ministry of Economic Affairs and Industry Co-operative Cooperatives of China is applicable to the Chinese National Standard (CNS) A4 specifications (210 X 297 mm) II A7 B7 C7 D7 VI. Patent application Ci_C6) Alkoxycarbonyl group and Nitro group; R1 is phenyl, c 〇2R2, S 〇2NHR3 or C ON R4R5, wherein R2 is selected from hydrogen and (Ci-C6) alkyl, R4 and R5 are selected from nitrogen (C3-Cl2) , 1 -— (Cl—C3) alkyl— (Cs_C8) cycloalkyl, and adamantyl, and R3 is (Cl—C6) alkyl: and w is hydrogen, chlorine Methyl; or a pharmaceutically acceptable salt thereof. 2 _ A compound according to item 1 of the patent application, wherein the compound is a compound of formula I in which Y1 and Y2 are both phenyl or one of Y1 and Y2 is cyclohexyl, or an pharmaceutically acceptable salt. \ 3 · The compound as claimed in item 1, wherein the compound is a compound of formula II in which Y1 is phenyl, or a pharmaceutically acceptable salt thereof. Wherein the compound is selected from the group consisting of: '2 — [3 — (3- (3-thiomethylphenyl) ureido) — 2-oxo — 5-phenyl — 2, 3, 4, 5-tetrahydro -1H-(1) benzodiazepine-1-yl] tert-butyl acetate; '3-— ((3-chlorophenyl) ureido) -7-cyclohexyl- (Nt-butoxycarbonylmethyl ) Hexahydroleatherine 2-ketone; 3- ((3-tolyl) ureido)-7-cyclohexyl one (Nt; butoxycarbonylmethyl) hexahydroazale leather 2-ketone; 3- ((3-Phenylphenyl) urea group)-7-cyclohexyl one (N-clothing paper scale is applicable to the China standard (CNS> A 4 specifications (210 X 297 mm> -------- ------- &lt; ------- installed ------ order ----- f line (please first «18 ^ surface precautions and then f this page) Hydrocarbon Economy Department Central Printed by the Bureau of Standards and Employee Consumer Cooperatives 3? A7 B7 C7 D7 6. Patent application scope 1 Adamantaneoxycarbonylmethyl) hexahydronitrogen Leather 1 '3 — ((3-Phenylphenyl) ureido) — 7 2 —adamantyloxycarbonylmethyl) hexahydroazazepine 1 — ((3 — tolyl) ureido) — 7 1 one diamond Alkoxycarbonylmethyl) hexahydroazaza leather 3 — ((3-tolyl) ureido) 7 2 —adamantyloxycarbonylmethyl) hexahydroazaza leather 3 — ((3 — methoxy Phenyl) ureido) -t-butoxycarbonylmethyl) hexahydroazepine leather-2 ((3-methoxyphenyl) ureido) -1 adamantaneoxycarbonylmethyl) hexahydroazepine leather 2-ketone: one cyclohexyl-2-ketone; one cyclohexyl-2-ketone; one cyclohexyl-2-ketone; 7—cyclohexyl-ketone; 7—cyclohexyl-2-ketone: (N (N-(N (N -(N (Please read the precautions on the back before writing this page)-Installed 3-((3 -methoxyphenyl) ureido) a 7 -cyclohexyl 2 -adamantyloxycarbonylmethyl) six Hydrazine leather 2-ketone; (N set 'ureido group) N — third butyl 2-5-phenyloxy [3 2, 3, (3, a methoxyphenyl) 4, 5 _ four 氲1H — (1) benzodiazepine-1 monoyl] acetamide acetate: N The third butyl 2- (3) urea group) oxyphenyl printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy 1H — (1) benzoazepine leather 1 'N, N — bis (2-propyl) benzene Radical) ureido) hydrogen-1HNHphenyl), ureido 2-oxo-5-(3- (3-thiomethylphenyl-2,3,4,5--yl) acetamide acetate; 2- [3- (3- (phenyl-2,3,4, tetrahydro-3-chloro5-tetra) benzoazepine-1-yl] acetamide acetate (2-propyl) 2- [ 3 — (3 — (2 one oxygen_ 5 — phenyl-2, 3, 4, 3—A 5—Four paper rulers and shoulders are suitable for China National Standards (CNS) A 4 specifications (210 X 297 y 炷) A7 B7 C7 D7 6. Scope of patent application (please read the precautions on the back before writing this page) Qi-1 1 Η-(i) benzodiazepine-1_yl] acetamide acetate:, 'N, N — Bis (2-propyl) 2- [3- (3- (3-methoxyphenyl) adenyl) -2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H- ( 1) Benzoazepine-1-yl] acetamide acetate; "1 ^, &gt; 1-bis (2-propyl 2— [3_ (3- (3-thiomethylphenyl) adenyl) -2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H— (1) benzodiazepine leather _1_yl] acetamide acetate: '2-[3-(3-(3-gas phenyl) ureido)-2-oxygen-5-phenyl-2, 3, 4, 5-tetrahydro-in — (1) Benzene gas leather 1-yl] tertiary butyl acetate: butyl: tertiary butyl 2- [3- (3- (3-tolyl) ureido) -2-oxo-5- Phenyl-2,3,4,5-tetraargon-1H— (1) benzoazepine-1-yl] tert-butyl acetate; and * 2-[3 — (3 — (3-methoxy Phenyl) ureido) -2-oxo-5-phenyl-2,3,4,, 5-tetrakis-1H- (1) benzodiazepine-1-yl] tert-butyl acetate. Du Printed by the Ministry of Economic Affairs Central Bureau of Standards for Consumer Consumption 5. A medical combination used to treat or prevent breast milk from diseases including pain, gastrointestinal disorders such as ulcers and colitis, and central nervous system disorders such as anxiety and fear Substances, which include an amount effective to prevent or treat this condition, such as the compound of patent application No. 1 compound, and a pharmaceutically acceptable carrier. 6. A pharmaceutical composition for antagonizing the action of cholecystokinin in the breast of hips, which includes the compound as claimed in item 1 of the patent application and its pharmaceutically acceptable carrier that can effectively antagonize CCK-B. Heart · A7 B7 C7 ----- D7 7T, patent application group 7 V—a compound of the formula Where R2 is hydrogen, phenyl, CO2R2, S〇2NR3R6 or CO R4R5, wherein the phenyl group can be freely selected from one or two groups each selected from halo, (Ci-C6) alkyl, (Ci-Ce) Alkoxy, nitro, amine and trifluoromethyl group substituents, and wherein R2, R3, R4, R5 and R6 are each selected from hydrogen, (C3-C12) alkyl and fused, saturated Carbocyclic system containing two or three rings; R8 is bromine, amine or azido; and Y1 is selected from phenyl, (C3-C8) linear or branched alkyl and (C5-C8) cycloalkyl Group, wherein the phenyl group can be freely selected from one or two substituents each selected from halo, (Ci-Cs) alkyl, (Ci-C6) alkoxy, nitro, amine, and trifluoromethyl Substituted, and wherein the cycloalkyl can be optionally substituted with one or two substituents each selected from (Ci-Ce) alkyl. ------------- {----: ------ installed ------ ΤΓ ----- LINE <Please read the precautions on the back before filling This page) Ministry of Economy Central Standard 4 Employee Consumer Cooperation Du Printed Attachment 1A: Chinese Patent Application No. 81110044 'Chinese Supplementary Pharmacology Tests, Substitutes and Substitutes: Me: methyl i # jT_ ί 楠 充 L ,. „This Nian Dan Et: · ethyl ifr: isopropyl t-butyl, tBu: third butyl tr-amyl: third 戍 基 _cjcl ohexy 1: 毩 hexyl t-octyl: third _ base Ada: Jin Gangyuan The Republic of Korea in 1992 5 Ph: benzyl: Monthly Amendment R z R IC «〇. NM CCK-B * 3-CH3 7-Ph C02tBu 120 3-CH3 7-t-butyl C02tBu 670 3-CH3 6,7-diPh C02tBu 333 3-CH3 7-Ph CH2Ph 200 3- CH3 7-Ph co2h 670 3-CH3 7-Ph CO CO2-Ada 660 3-CH3 7-Ph 00N 0 540 3-CH3 5-Ph CH2Ph 700 3-CH3 7-Ph CONHt-octyl 300 3-CH3 7- Ph CONH-1-Ada 2,200 3-CH3 5-tBu C02tBu 440 3> CH3 7- (4-F) Ph C02tBu 430 3-CH3 7, Ph C〇2_2-Ada 82 3-CH3 7-cyclohexyl C02tBu 16.6 3- CFg 7-cyclohexyl C02tBu 56.9 3-CH3 7-benzyl C02tBu 50 3-CI 7-benzyl C〇2tBu 74 3-CH3 5,7-diPh C02tBu 10.45 3-F 5,7-diPh C02tBu 550 3-Et 5,7 -diPh C02tBu 120 3-OMe 5,7-diPh C02tBu 9.8 Our guinea pig cortical replacement 125 丨 -GGK-8 ^ 6/10 3 3 3 Η I Η Ηc c c C I · ι ·· 3 4 3 3 C02tBu 3.5 C02tBu 24 co2h 100 Ph 36 3-CH3 CONHtBu 1.3 3-CI CONHtBu 2.9 2-CH3 CONHtBu 28.7 3-OCH3 CONHtBu 7.21 4-CI CONHtBu 22.3 4-CH3 CONHtBu 17-9 3-CF3 CONHtBu 13.8 3-SCH3 CONHtBu 1.7 * from guinea pig cortex replacement 125l-CCK -8; 5- 3-33: 11:40; PATENT PFIZER INC;? 7/10 ARTMENT- 3-CH3 3-CI 3-CH3 3-CH3 3-Cl 3-CH3 3-CH3 3-CH3 3-CI 3ΌΗ3 3-CH3 3-CH3 3-CH3 3-CH3 3-Et 3-NMe2 3-C02Et 3 -C〇2Me 3-C02H 3-CH3 X ζ Η 7-CH3 7-CH3 Η Η Η 3 3 3 3 3 3 3 3 3 Η Η Η I ι Η Η Η Η Η Η cccc CCCCCCC-· -ιιι- · __- &quot; · Η8897ΗΗ8888888 2-CI Η Η 3,4-diCI 4-CH3 4-F 2- F Η Η Η Η 3- CI 4- CF3 Η Η Η Η Η Η 3-CH3 \ Cs〇, m , CCK-B '240 44 14 48 1.1 18 5.8 0.6 20 70 140 5.8 0.66 0.83 2.8 0.97 2.0 2.0 * From guinea pig 12sI-CCK-8 3 i • PFIZER h \ C; 5- 3-93; 11:40: PATENT DEPARTMENT- »8/10 i X ugly 1 B2 ICKn. NM. CCK-B 3-CH3 ch3 t-Bu 0.5 3-CI ch3 t-Bu 0.7 2.6 3-CH3 H t-amyl 3-CH3 H (l-Me) cyclohexyl 9.3 3-CH3 HC {CH3) 2Ph 19 CCK-B 丨 C50, nM B CH2Ph 210 CH2 cyclohexyl 87 cyclohexyl 5.3 * Replaced from guinea pig cortex 125l-CCK-8 4; # 9/10 Yu Pai "1 M -PFIZER INC; 5- 3-33; 11:41; PATENT DEPARTMENT · ^ CCK-B l £ s〇1 nM * 200 280 520 CH3 Σ H ch3 CCK-B ICgQ. NM 158.1 * Replacement from guinea pig cortex 125 | -CCK-8 5 h. \ R INC; 5- 3-33; 11:41; P; A Office \ TE \ T DEPARTMENT ”; #! 0 /! 0 z lCRn. nM CCK-B1 3-CH3 3-0Me 3-CH3 3-CI 3-CH3 3-NMe2 3-CH3 3-NO2 3-NHAc 3-NHS02CH3 3-CH3 3-CH3 3-iPr 3-0Me 3-CH3 3-CH3 3- CH3 3- SCH3 4- CH3 3- CN 2- CH3 4- CI 3,4-diCH3 3- CH3,4-CI 3 3 丨 Η HF ccc — --i H 4 4 4 3 H 3-0 Me Η Η Η 3-F Η Η Η Η Η Η Η Η Η Η Η Η Η HHHHHHHHHHHH 4-FH 4-CH3 4-CH3 2- CH3 3- CH3 H H H H H H H 26 80 65 730 200 3.6 210 17 120 110 31 66 32 190 69 7,8 68 38 41 17 180 28 52 60 6 1 Replaced by guinea pig cortex 125 丨 _CCK_8.