IL33889A - Preparation of 7-amino cephalosporin esters - Google Patents

Preparation of 7-amino cephalosporin esters

Info

Publication number
IL33889A
IL33889A IL33889A IL3388970A IL33889A IL 33889 A IL33889 A IL 33889A IL 33889 A IL33889 A IL 33889A IL 3388970 A IL3388970 A IL 3388970A IL 33889 A IL33889 A IL 33889A
Authority
IL
Israel
Prior art keywords
acid
hydrogen
formula
solvent
compound
Prior art date
Application number
IL33889A
Other versions
IL33889A0 (en
Original Assignee
Lilly Co Eli
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lilly Co Eli filed Critical Lilly Co Eli
Publication of IL33889A0 publication Critical patent/IL33889A0/en
Publication of IL33889A publication Critical patent/IL33889A/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D501/00Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
    • C07D501/14Compounds having a nitrogen atom directly attached in position 7
    • C07D501/16Compounds having a nitrogen atom directly attached in position 7 with a double bond between positions 2 and 3
    • C07D501/187-Aminocephalosporanic or substituted 7-aminocephalosporanic acids
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/55Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Cephalosporin Compounds (AREA)

Description

PREPARATION OF 7-AMINO CEPHALOSPORIN ESTERS The present invention provides a process for preparing 3-methyl-7-amino cephalosporin compounds from 3-methyl-7-acylamido cephalosporin compounds.
More particuJa rly, the present invention provides a process for preparing a compound having the formula C02R' which comprises treating a compound having the formula C02R' with at least one mole of a solvent having the formula R"-0H at a temperature within the range of 0* to 125°C. in the presence of at least 0.25 equivalent of an acid having a pjCa of less than 3, wherein or Q is hydrogen, to alkyl, to alkoxy, cyano, nitro h drox chloro bromo or fluoro Y is hydrogen or hydroxy; X is oxygen or sulfur; m is an integer of 0 to 2; n is an integer of 1 to 3; 2, 2, 2-trichloroethyl or p-nitrobenzyl; and R* is hydrogen or an easily removable oarboxyl pr-oteoting group, — a«d- R" is hydrogen, methyl, ethyl, or propyl.
R may be such groups as benzyl, m-chlorobenzyl, p-cyanobenzyl, a-hydroxybenzyl, a-hydroxy-o_-ethylbenzyl, phenoxymethyl, benzyloxymethyl, £-nitrobenzyloxymethyl, phenoxyethyl, thiophenoxyethyl, £-methylthiophenoxyethyl, and p-methoxybenzyloxyethyl. This process will find its greatest application with those compounds wherein R is benzyl or phenoxymethyl, since such compounds can be obtained from penicillin G and penicillin V by the Morin- 626 Jackson process described in U.S. Patent 3.» 275,636-.
The carboxyl group in the starting material for this process may be present as the free acid but is preferably ester if led by an easily removable carboxyl protect -ing group. It is well known to protect a carboxyl group by esterlfication with a group that can be easily removed by acid hydrolysis or hydrogenolysis . Examples of such groups include 2, 2, 2-trichloroethyl, bonnylj bonahydryl, p-nitrobenzyl, triroethylsllyJi, phthalimidomethyl, succln-lmidomethylj phenaoylj 2- (2-methy.L-3-butynyl) } and 2-(2 mothyl 3-butenyl). The particular carboxyl protecting group employed is unimportant and does not affect the process except that a carboxyl protecting group that can be removed by acid hydrolysis may be removed during the course of this process so that the product would contain - ceptable since the free carboxyl group will not interfere with this process.
In accordance with this process the acylated cephalosporin starting material is treated with a molar excess of water or a lower alkanol such as methanol, ethanol, or propanol. Water is preferred. It appears that a solvolysis of the amide linkage occurs with the formation of the free amine and an acid when water is the solvent or an ester when an alcohol is the solvent. It is to be understood of course that mixtures of these solvents may be used. At least one mole of the reactive solvent should be used per mole of starting cephalosporin compound. It is preferred to use an excess of the reactive solvent, and this is usually done. Any excess may be used limited only by the equipment needed to separate the products of the reaction from the excess solvent. When water is the sole reactive solvent it is preferred to use an inert organic co-solvent to aid in maintaining starting materials and products in solution. This co-solvent should be miscible with water. Suitable co-solvents include tetrahydrofuran, dioxane, acetone, dlmethylsulf-oxide, acetonitrile, dimethylformamide, and dimethyl-acetamide.
The reaction between the acylated cephalosporin and the reactive solvent is conducted in the presence of a strong acid having a pKa of less than 3. This acid may be a mineral acid or an organic acid. Examples of such acids include p-toluenesulfonic acid, methanesulfonic acid, tri-fluoroacetic acid, hydrochloric acid, sulfuric acid and phosphoric acid. The preferred acid is p-toluenesulfonic ated cephalosporin should be used and preferably one equivalent or more of acid is used. As much as a 20 to 25 fold excess of acid may be employed but such excesses are unnecessary.
The reaction may be conducted at a temperature within the range of 0° to about 125° C. The preferred temperature is 25° to 75°C. The time of the reaction is a function of the acid employed, the solvent employed, and the temperature.. The time will normally be from about 1 to about 60 hours and will usually be less than 12 hours , The process will be further illustrated by the following examples.
Example 1 A solution of 20 g. of p-nitrobenzyl 3-methyl-7-phenoxyacetamido- -cephem-4-carboxylate and 16 g. of p-toluenesulfonic acid monohydrate in 16 ml. of water and 70 ml. of tetrahydrofuran was stirred and heated under reflux for a period of 3 hours. At the end of this time 5 ml. of water was added and the mixture was stirred and chilled in an ice bath for one-half hour. The solid that precipitated was filtered, rinsed with a cold 1:1 mixture of tetrahydrofuran and water and vacuum dried. This solid was 10.5 g. of unreacted starting material. The total filtrate from above was stripped of tetrahydrofuran on a rotary evaporator. The solid that precipitated during the stripping was filtered and rinsed with cold two percent aqueous p-toluenesulfonic acid solution. This solid was pulled damp dry on the filter, washed twice with 10 ml. portions of isopropyl acetate, and air dried to - - - - - - - -carboxylate £-toluenesulfonlc acid salt monohydrate.
The procedure of Example 1 was repeated using different acids and different solvent systems. The results are summarized in Table 1.
Table 1 Acid Temp., Time Acid Cone 'n. Solvent eC. hrs.
HC1 1.2M 4 ml. ¾0 66 5 ml. THP TgOH 1.3 5 ml. H20 57 7 ml. (CH3)2C0 HpSO.. 1.8M 4 ml. H 0 5# 66 10 ml. THP MeSO_H 1.3M 5 ml. ¾0 # 66 6 -5 20 ml. THP T OH 1.3M. 3 ml. ¾0 # 65 6 ml. CH3C1 TgOH 1.3M 5 ml. H2O # 100 1 ml. DMSO TgOH = p-toluenesulf onic acid MeSO^H = methanesulf onic acid THP = tetpahydrof uran DMSO = dimethyls ulf oxide Another series of reactions was run following the procedure of Example 1 except that the starting material was 2,2,2-trlchloroethyl 3-raethyl-7-phenoxyacet-amldo- cephem-4-carbox late. The results of these runs are summarized In Table 2.
Table 2 Moles Acid Amide Temp., Time, Acid Moles Amide Solvent Conc'n.,# °C. Hrs . Yield, % HC1 20 CH30H 0.6 -^27 20 47 HC1 4 CH30H ¾7 15 52 T„OH 2.5 CH30H 5 45 22 58 TsOH 1 CH^OH 5 65 5 57 TsOH 1 C¾0H 5 65 12 52 TsOH 2.5 C9H 0H 5 78 4 38 TeOH 12.5 C¾0H 5 75 1.75 5 T OH 12.5 5 66 .5 68

Claims (5)

1. A process for preparing a compound having the formula 0=C - N ,C-CH, (I) \ c✓ 3 C02R< which comprises treating a compound having the formula C02R» with at least one mole of a solvent having the formula R"-OH at a temperature within the range of 0" to 125°C. in the presence of at least 0.25 equivalent of an acid having a PKa of- less than 3, wherein or Q is hydrogen, Cj. to alkyl, Cj. to alkoxy, cyano, nitra, hydroxy, chloro, bromo, or fluoro; Y is hydrogen or hydroxy; X is oxygen or sulfur; m is an integer of 0 to 2; n is an integer of 1 to 3; 2, 2, 2 -trichloroethyl or p-nitrobenzyl; and R* is hydrogen or an easily removable oarboxyl protect lng group j and R" is hydrogen, methyl, ethyl, or propyl.
2. The process of claim 1 wherein R is benzyl or phenoxymethyl.
3. The process of claim 2 wherein R" is hydrogen, the acid is p-toluenesul onic acid, and the temperature is within the range of 25° to 75° C.
4. The process for preparing 3 -me hyl -7 -amino cephalosporin compounds, substantially as herein described with particular reference to any one of the specific examples. of Formula I in claim 1, whenever
5. The compounds/ obtained by the process of any of claims 1 to 4. 8. HOROWITZ * CO. Agente lor Applicant*
IL33889A 1969-03-10 1970-02-12 Preparation of 7-amino cephalosporin esters IL33889A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US80582369A 1969-03-10 1969-03-10

Publications (2)

Publication Number Publication Date
IL33889A0 IL33889A0 (en) 1970-04-20
IL33889A true IL33889A (en) 1973-04-30

Family

ID=25192601

Family Applications (1)

Application Number Title Priority Date Filing Date
IL33889A IL33889A (en) 1969-03-10 1970-02-12 Preparation of 7-amino cephalosporin esters

Country Status (13)

Country Link
JP (1) JPS4931999B1 (en)
AT (1) AT293620B (en)
BE (1) BE746860A (en)
CA (1) CA974516A (en)
CH (1) CH529788A (en)
DE (1) DE2010757A1 (en)
ES (1) ES377228A1 (en)
FR (1) FR2037887A5 (en)
GB (1) GB1266252A (en)
IE (1) IE33722B1 (en)
IL (1) IL33889A (en)
NL (1) NL7003048A (en)
SE (1) SE374374B (en)

Also Published As

Publication number Publication date
IL33889A0 (en) 1970-04-20
GB1266252A (en) 1972-03-08
IE33722L (en) 1970-09-10
CH529788A (en) 1972-10-31
BE746860A (en) 1970-09-07
NL7003048A (en) 1970-09-14
IE33722B1 (en) 1974-10-02
AT293620B (en) 1971-10-25
ES377228A1 (en) 1972-06-01
FR2037887A5 (en) 1970-12-31
CA974516A (en) 1975-09-16
JPS4931999B1 (en) 1974-08-27
SE374374B (en) 1975-03-03
DE2010757A1 (en) 1970-09-17

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