CS214360B1 - Novel 0-/2-chlorethyl/0-alkyl/n-alkylamido/esters of chlorthiophophoric acid and method production the same - Google Patents

Novel 0-/2-chlorethyl/0-alkyl/n-alkylamido/esters of chlorthiophophoric acid and method production the same Download PDF

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CS214360B1
CS214360B1 CS841480A CS841480A CS214360B1 CS 214360 B1 CS214360 B1 CS 214360B1 CS 841480 A CS841480 A CS 841480A CS 841480 A CS841480 A CS 841480A CS 214360 B1 CS214360 B1 CS 214360B1
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chloroethyl
toluene
formula
analysis
alkyl
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Vaclav Konecny
Jozefina Wolfshoerndlova
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Vaclav Konecny
Jozefina Wolfshoerndlova
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Predmetom vynálezu sú nové 0-/2-chlóretyl/0-alkyl/N-alkylamido/ estery kyseliny chlórtiofosforečnej a sposob ich přípravy. Uvedené zlúčeniny je možné použit' ako medziprodukty pri ^syntéze esterov kyseliny tiofosforečnej.The present invention relates to novel O- (2-chloroethyl) O-alkyl (N-alkylamido) chlorothiophosphoric esters and processes for their preparation. These compounds can be used as intermediates in the synthesis of thiophosphoric acid esters.

Z literatúry sú známe 0-/2-fluóretyl/0-etyl ester kyseliny chlórtiofosforečnej, ktorý sa připravuje z 0-/2-fluóretyl/dichlórtiofosfátu a etylalkoholu za přítomnosti trietylamínu a 0-/2-fluóretyl/-metyl chlórtiofosfonát, ktorý sa připravuje reakciou metyl dichlórfosfónovej kyseliny 2-fluóretanolu v přítomnosti trietylamínu /2.obšč.chim. 29, 1671 /1959//. Taktiež sú známe O-/chlórallyl/S-alkyl, aryl, aralkylchlórtiofosfáty /Pat. SSSR 566.847/.Chlorothiophosphoric acid O- (2-fluoroethyl) O -ethyl ester, which is prepared from O- (2-fluoroethyl) dichlorothiophosphate and ethyl alcohol in the presence of triethylamine and O- (2-fluoroethyl) methyl chlorothiophosphonate, is prepared from the literature by the reaction of methyl dichlorophosphonic acid 2-fluoroethanol in the presence of triethylamine (2 nd). 29, 1671 (1959). O- (chloroallyl) -S-alkyl, aryl, aralkylchlorothiophosphates (Pat) are also known. USSR 566,847 /.

Teraz sa zlstlli nové 0-/2-chlótetyl/0-alkyl/N-alkylamido/ estery kyseliny chlórtiofosforečnej všeobecného vzorca IThe novel O- (2-chloroethyl) O-alkyl (N-alkylamido) chlorothiophosphoric esters of formula I

v ktorom R1 znamená alkyl s 1 až 4 atómami uhlíka, X znamená kyslík alebo -NH skupinu.wherein R 1 is C 1 -C 4 alkyl, X is oxygen or -NH.

Súčasne sa zlstil sposob přípravy zlúčenín všeobecného vzorca I reakciou O-/2-chlóretyl/ /dichlórtiofosfátu vzorce IIAt the same time, the process for the preparation of the compounds of the formula I by reaction of O- (2-chloroethyl) -dichlorothiophosphate of the formula II

214 360214 360

214 360214 360

Cl - CH2 Cl - CH 2

/11/ s alkalickým alkoholátom všeobecného vzorce III(11) with an alkali alcoholate of formula III

R1 - OM /111/ v ktorom R1 má už uvedný význam, M znamená alkalický kov ako je sodík, draslík, alebo s amínom všeobecného vzorca IVR 1 - OM / 111 / in which R 1 is as instructions listed above, M is an alkali metal such as sodium, potassium, or with an amine of formula IV

R1 - NH2 /IV/ v ktorom R1 má už uvedený význam v prostředí inertného organického riedidla pri teplote -5 až 25 °C.R 1 - NH 2 (IV) wherein R 1 is as previously defined in an inert organic diluent at -5 to 25 ° C.

Zlúčeniny pódia vynálezu vzorca I možno tiež pripraviť reakciou zlúfeniny všeobecného vzorca VCompounds of the invention of formula I may also be prepared by reaction of a compound of formula V

s 2-chlóretanolom za přítomnosti činidla viažúceho vznikajjúci chlorovodík ako je trietylamín, pyridin v prostředí inertného organického riedidla pri teplote O až 25 °C.with 2-chloroethanol in the presence of a hydrogen chloride-forming agent such as triethylamine, pyridine in an inert organic diluent at 0-25 ° C.

Následujďce příklady bližšie osvetíujú ale neobmedzujú nové O-/2-chlóretyl/O-alkyl/N-alkylamido/ estery kyseliny chlórtiofosforečnej a sposob ich přípravy.The following examples illustrate but do not limit the novel O- (2-chloroethyl) O-alkyl (N-alkylamido) chlorothiophosphoric esters and methods for their preparation.

Příklad 1Example 1

0-/2-chlóretyl/0-izobutylchlórtiofosfát0- / 2-chloroethyl / 0-izobutylchlórtiofosfát

K 1 molu 0-/2-chlóretyl/dichlórtiofosfátu rozpuštěného v 600 ml toluénu sa za miešania přidalo v priebehu 120 min. 1,05 molu izobutylátu draselného, rozpuštěného v 100 ml izobutanolu a v 150 ml toluénu, pri teplote O až 8 °C. Po přidaní sa pokračovalo v miešaní ešte 3 hodiny bez chladiacej lázně. Potom sa reakčná zmes premyla 3 x 500 ml vody, vysušila sa a za zníženého tlaku sa oddestiloval toluén s izobutanolom. Destilačný zvyšok sa predestiloval za zníženého tlaku. Získalo sa: 239,5 .g bezfarebnej kvápaliny o t.v. 75-77 °C/26,7Pa n20 . χ,49χ3 a zloženia:To 1 mole of O- (2-chloroethyl) dichlorothiophosphate dissolved in 600 mL of toluene was added over 120 min with stirring. 1.05 mol of potassium isobutylate, dissolved in 100 ml of isobutanol and 150 ml of toluene, at 0 to 8 ° C. After the addition, stirring was continued for 3 hours without cooling bath. Then, the reaction mixture was washed with water (3 x 500 ml), dried and toluene with isobutanol distilled off under reduced pressure. The distillation residue was distilled under reduced pressure. Yield: 239.5 g of a colorless liquid of 75-77 ° C / 26.7 Pa n 20. χ, 49χ3 and composition:

Analýza pre CgH^Cl^PS Vyp.: 12,34 % P 12,77 % S 28,24 S Cl /m.h. 251,02/ Zist.: 12,11 %P 13,08 % S 28,48 % Cl.Analysis for C 8 H 11 Cl 2 PS Calc .: 12.34% P 12.77% S 28.24 S Cl / m.h. Found: 12.11% P 13.08% S 28.48% Cl.

Struktúra zlúčeniny bola potvrdená IC spektroskopidou.The structure of the compound was confirmed by IC spectroscopy.

Ič spektrá v CC14 = V/P S/ s 695 cm-1 ^/Cl-C / : 582 cí1 ^/P-O-C/ : 895>970;985;1055;1100 cm“1.IR spectra of CC1 4 = W / PS / 695 cm s -1 ^ / C-C / 582 CI 1 ^ / POC / 895> 970, 985, 1055, 1100 cm '1.

Podobným postupom boli připravené zlúčeniny:The following compounds were prepared in a similar manner:

O/2-chlóretyl/O-metylchlóreiofosfát n20 = 1,5037 t.v. = 65 °C /13,4 PaO / 2-chloroethyl / O-methylchlorophosphate n 20 = 1.5037 tt = 65 ° C / 13.4 Pa

DD

214 360214 360

Analýza pre C^Cl^PS Vvp.: 14,82 % P 15,34 % S 33,93% Cl, /m.h. = 208,97/ Zist.j 14,42%P 15,98 % S 33,44 % Cl.Analysis for C ^ Cl Cl ^ ^ PS PS Vp: 14.82% P 15.34% S 33.93% Cl, m / h. = 208.97 / found 14.42% P 15.98% S 33.44% Cl.

Q-/2-chlóretvl/0-etylchlórtiofosfát n^0 = 1,5002 t.v. : 80 - 82 °C/121 PaQ- (2-Chloroethyl) -O-ethylchlorothiophosphate n = 0 = 1.5002 tv: 80 - 82 ° C / 121 Pa

Analýza pre C4HgCl2O2PS Vyp.: 31,80 % Cl 13,88 % P 14,31 % S, /m.h.-- 222;98/Analysis for C 4 H 9 Cl 2 O 2 PS Calc .: 31.80% Cl 13.88% P 14.31% S, / mh-- 222; 98 /

Zist.: 31,66 % Cl 14,10 % P 14, 62 % SFound: 31.66% Cl 14.10% P 14, 62% S

0-/2-chlóretyl/0-izo-propylchlórtiofosfát n20 » 1,4962 t.v. : 75 °C /53,4 Pa0- (2-chloroethyl) O-iso-propylchlorothiophosphate n 20 »1.4962 t: 75 ° C / 53.4 Pa

Analýza pre C5HUC12O2PS Vyp.: 29,91 % Cl 13,06 % P 13,49 % S , /m.h. '» 236,99/Analysis for C 5 H U Cl 2 O 2 PS Calc .: 29.91% Cl 13.06% P 13.49% S, / mh »» 236.99 /

Zist.: 30,16 % Cl 13,22 % P 13, 62 % S.Found: 30.16% Cl 13.22% P 13, 62% S.

Příklad 2Example 2

0-/2-chlóretyl/0-izobutylchlórtiofosfát0- / 2-chloroethyl / 0-izobutylchlórtiofosfát

K 1 molu O-izobutyldichlórtiofosfátu rozpuštěného v 600 ml v toluénu sa za miešania pri teplote 5 až 10 °C přidalo 1ÍO5 molu 2-chlóretanolu a 1,05 molu trietylamínu.Po přidaní oboch látok sa pokračovalo v miešaní 8 hodin pri teplote 40 °C. Potom sa reakčná zmes ochladila, premyla 3 x 500 ml vody. Toluénový roztok sa vysušil a toluén sa oddestiloval za zníženého tlaku. Destilačný zvvšok sa nredestiloval za zníženého tlaku. Získala sa zlúčenina o t.v. - 75-77 °C/26,7 Pa, ktorá je identická so zltíčeninou v příklade 1.To 1 mole of O-isobutyldichlorothiophosphate dissolved in 600 ml in toluene was added 10 mole of 2-chloroethanol and 1.05 mole of triethylamine while stirring at 5-10 ° C. After the addition of both substances, stirring was continued at 40 ° C for 8 hours. . Then the reaction mixture was cooled, washed with 3 x 500 mL water. The toluene solution was dried and the toluene was distilled off under reduced pressure. The distillation residue was not distilled under reduced pressure. A compound of b.p. - 75-77 ° C / 26.7 Pa, which is identical to the compound of Example 1.

Příklad 3Example 3

0-/2-chlóretyl/N-izobutylamldochlórtlofosfát0- / 2-chloroethyl / N izobutylamldochlórtlofosfát

K 0,5 molu 0-/2-chlóretyl/dichlórtiofosfátu v 300 ml toluénu sa za miešania přidalo 1,05 molu izobutylamínu v 100 ml toluénu pri teplote - 6 až 0 °C počas 90 minút. Po přidaní sa reakčná zmes miešala 2 hodiny bez lázně, potom sa premyla 3 x 300 ml vody, vysušila sa bezv. chloridom vápenatým. Toluén sa oddestiloval za zníženého tlaku a destilačný zvyšok sa predestiloval za vákua. Získalo sa 33, 3 g bezfarebnej kvapaliny t.v. 108 - 110 °C/26,7 Pa n20 « 1,5130To 0.5 mole of O- (2-chloroethyl) dichlorothiophosphate in 300 mL of toluene was added with stirring 1.05 mole of isobutylamine in 100 mL of toluene at -6 to 0 ° C for 90 minutes. After the addition, the reaction mixture was stirred for 2 hours without bath, then washed with 3 x 300 ml of water, dried without addition of water. calcium chloride. Toluene was distilled off under reduced pressure and the distillation residue was distilled under vacuum. 33.3 g of a colorless liquid were obtained at 108-110 ° C / 26.7 Pa n 20 «1.5130

DD

Analýza pre: CgH^Cl^JOPS : Vyp.: 28,35 % Cl 12,38 % P Zist.: 28,78 % Cl 12,82 % P 13, 01 % S. štruktúra zlúčeniny bola potvrdená IČ spektroskópiou.Analysis for: C 8 H 11 Cl 2 JOPS: Calc .: 28.35% Cl 12.38% P Found: 28.78% Cl 12.82% P 13.01% S. The structure of the compound was confirmed by IR spectroscopy.

12,82 % S, /m.h.12.82% S, m / h.

250,12/250.12 /

Ič spektrá v CC14 Spectrum in CC1 4

7P S/ J/C - Cl/ ýp-o-c/ % - H /7P S / J / C - Cl / pp-oc /% - H /

665 a 692 cm665 and 692 cm

570 cm570 cm

887; 955;972:1O5O a 1105 cm'887; 955; 972: 1050 and 1105 cm -1

3430 cm3430 cm

Claims (3)

3 214 360 Analýza pre C^Cl^PS Vvp.: 14,82 % P 15,34 % S 33,93% Cl, /m.h. = 208,97/ Zist.j 14,42%P15,98 % S 33,44 % Cl. Q-/2-chlóretyl/0-etylchlórtiofosfát n^0 = 1,5002 t.v. : 80 - 82 °C/121 Pa Analýza pre C4HgCl2O2PS Vyp.: 31,80 % Cl 13,88 % P 14,31 % S, /m.h.-- 222;98/ Zist.: 31,66 % Cl 14,10 % P 14, 62 % S 0-/2-chlóretyl/0-izo-pronylchlórtiofosfát n20 » 1,4962 t.v. : 75 °C /53,4 Pa Analýza pre Cgl^Cl^PS Vyp.: 29,91 % Cl 13,06 % P 13,49 % S , /m.h. '» 236,99/ Zist.: 30,16 % Cl 13,22 % P 13, 62 % S. Příklad 2 0-/2-chlóretyl/0-izobutylchlórtiofosfát K 1 molu O-izobutyldichlórtiofosfátu rozpuštěného v 600 ml v toluénu sa za miešania pri tep-lotě 5 až 10 °C přidalo 1ÍO5 molu 2-chlóretanolu a 1,05 molu trietylamínu.Po přidaní obochlátok sa pokračovalo v miešaní 8 hodin pri teplote 40 °C. Potom sa reakčná zmes ochladila,premyla 3 x 500 ml vody. Toluénový roztok sa vysušil a toluén sa oddestiloval za zníženéhotlaku. Destilačný zvvšok sa predestiloval za zníženého tlaku. Získala sa zlúčenina ot.v. - 75-77 °C/26,7 Pa, ktorá je identická so zltíčeninou v příklade 1. Příklad 3 0-/2-chlóretyl/N-izobutylamidochlórtiofosfát K 0,5 molu 0-/2-chlóretyl/dichlórtiofosfátu v 300 ml toluénu sa za miešania přidalo 1,05 molu izobutylamínu v 100 ml toluénu pri teplote - 6 až 0 °C počas 90 minút. Po přidaní sa reakčná zmes miešala 2 hodiny bez lázně, potom sa premyla 3 x 300 ml vody, vysušila sa bezv. chlori- dom vápenatým. Toluén sa oddestiloval za zníženého tlaku a destilačný zvyšok sa predestiloval za vákua. Získalo sa 33, 3 g bezfarebnej kvapaliny t.v. " 108 - 110 °C/26,7 Pa n20 « 1,5130 D Analýza pre: CgH^Cl^JOPS : Vyp.: 28,35 % Cl 12,38 % PZist.: 28,78 % Cl 12,82 % P 13, 01 % S.štruktúra zlúčeninv bola potvrdená IČ spektroskópiou. 12,82 % S, /m.h. 250,12/ Ič spektrá v CC14 7P S/J/C - Cl/ýp-o-c/% - H / 665 a 692 cm 570 cm -1 887; 955;972:1O5O a 1105 cm' 3430 cm -1 -1 VYNALEZU3,214,360 Analysis for C ^ ClH ^ PSN VOv: 14.82% P, 15.34% S, 33.93% Cl, / m.h. = 208.97 / Found 14.42% P15.98% S 33.44% Cl. Q- (2-chloroethyl) O-ethylchlorothiophosphate n = 0 = 1.5002 t.o. : 80 - 82 ° C / 121 Pa Analysis for C 4 H 8 Cl 2 O 2 PS Off: 31.80% Cl 13.88% P 14.31% S, / mh - 222; 98 / Found: 31.66% Cl 14.10 % P 14, 62% S 0- / 2-chloroethyl / O-iso-pronylchlorothiophosphate n20 »1.4962 tv : 75 ° C / 53.4 Pa Analysis for Cgl 2 Cl 2 PS Off: 29.91% Cl 13.06% P 13.49% S, /m.h. ≪ tb > ______________________________________ < tb > ______________________________________ Example 2 O- / 2-Chloroethyl / O-isobutylchlorothiophosphate To 1 mole of O-isobutyldichlorothiophosphate dissolved in 600 ml in toluene under stirring at 5 to 10 ° C, 10 5 mol of 2-chloroethanol and 1.05 mol of triethylamine were added. After the addition of the dough, stirring was continued at 40 ° C for 8 hours. Then the reaction mixture was cooled, washed with 3 x 500 mL of water. The toluene solution was dried and toluene was distilled off under reduced pressure. The distillation residue was distilled under reduced pressure. The compound of formula I was obtained. - 75-77 ° C / 26.7 Pa, which is identical to that of Example 1. Example 3 O- (2-Chloroethyl) N-isobutylamidochlorothiophosphate To 0.5 mol of O- (2-chloroethyl) dichlorothiophosphate in 300 ml of toluene 1.05 mol of isobutylamine in 100 ml of toluene was added with stirring at -6 to 0 ° C for 90 minutes. After the addition, the reaction mixture was stirred without bath for 2 hours, then washed with 3 x 300 mL of water, dried in vacuo. calcium chloride. The toluene was distilled off under reduced pressure and the distillation residue was distilled under vacuum. 33.3 g of a colorless liquid were obtained. "108-110 ° C / 26.7 Pa n 2 O« 1.5130 D Analysis for C 8 H 11 Cl 2 JOPS: Off: 28.35% Cl 12.38% Purity: 28.78% Cl 12.82% P 13, 01% S. Structure of Compounds was confirmed by IR spectroscopy 12.82% S, / mh 250.12 / Ic spectra in CC14 7P S / J / C - Cl / β-oc /% - H / 665 and 692 cm 570 cm -1 887; 955; 972: 1O5O and 1105 cm '3430 cm -1 -1 FILLED 1. Nové 0-/2-chlóretyl/0-alkyl/N-alkylamido/ estery kyseliny chlórfiofosforečnej všeobecné- ho vzorca I 214 360 41. New O- (2-chloroethyl) O-alkyl (N-alkylamido) esters of chlorophosphoric acid of the general formula I 214 360 4 ci - ch2ch2-o Cl /1/ v ktorom R1 znamená alkyl s 1 až 4 atómami uhlíka, X znamená kyslík alebo -NH skupinu.in which R 1 is alkyl of 1 to 4 carbon atoms, X is an oxygen or -NH group. 2. Sposob přípravy zldčenín pódia bodu 1, vyznačený tým, že sa nechá reagovat! 0-/2-chlór- etyl/dichlórtiofosfát vzorca II2. A method for preparing a batch of step 1, characterized in that it is reacted! O- (2-chloroethyl) dichlorothiophosphate of formula II /11/ s alkalickým alkoholátem všeobecného vzorca III R1 - OM /111/ v ktorom R1 má už uvedený význam, M znamená alkalický kov ako je sodík , draslík,alebo s amínom všeobecného vzorca IV R1 - NH2 /IV/ v ktorom R1, má už uvedený význam v prostředí Inertného organického riedidla pri teplotě -5 až 25 °C.(11) with an alkali alcoholate of formula (III) R1 - OM / 111 / in which R1 is as defined above, M is an alkali metal such as sodium, potassium, or with an amine of formula IV R1 - NH2 / IV / in which R1 has as defined above in an inert organic diluent at -5 to 25 ° C. 3. Sposob přípravy zldčenín podťa bodu 1 vyznačený tým, že sa nechá reagovat* zldčenina vše- obecného vzorca V3. A process for preparing compounds according to claim 1, wherein the compound of formula (V) is reacted. /V/ v ktorom R1 má už uvedený význam 2-chlóretanolom za přítomnosti činidla viaždceho vznikajdci chlorovodík ako je trietyl-amin, pyridin, v prostředí inertného organického riedidla pri teplote O až 25 °C. Cena: 2,40 Kčs Vytiskly Moravské tiskařské závody, provoz 12, Leninova 21, OlomoucWherein R 1 is as defined above with 2-chloroethanol in the presence of a hydrogen chloride reagent such as triethylamine, pyridine, in an inert organic diluent at 0 to 25 ° C. Price: 2,40 Kčs Printed by Moravské tiskařské závody, operation 12, Leninova 21, Olomouc
CS841480A 1980-12-03 1980-12-03 Novel 0-/2-chlorethyl/0-alkyl/n-alkylamido/esters of chlorthiophophoric acid and method production the same CS214360B1 (en)

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