SU475363A1 - Method for producing chlorocycloalkyltriothiophosphonic acid thioanhydrides - Google Patents

Method for producing chlorocycloalkyltriothiophosphonic acid thioanhydrides

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Publication number
SU475363A1
SU475363A1 SU1964276A SU1964276A SU475363A1 SU 475363 A1 SU475363 A1 SU 475363A1 SU 1964276 A SU1964276 A SU 1964276A SU 1964276 A SU1964276 A SU 1964276A SU 475363 A1 SU475363 A1 SU 475363A1
Authority
SU
USSR - Soviet Union
Prior art keywords
chlorocycloalkyltriothiophosphonic
producing
acid
hydrogen sulfide
thioanhydrides
Prior art date
Application number
SU1964276A
Other languages
Russian (ru)
Inventor
Октябрина Николаевна Гришина
Николай Андреевич Андреев
Эльвира Ивановна Бабкина
Original Assignee
Ордена Трудового Красного Знамени Институт Органической И Физической Химии Им.А.Е.Арбузова
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Application filed by Ордена Трудового Красного Знамени Институт Органической И Физической Химии Им.А.Е.Арбузова filed Critical Ордена Трудового Красного Знамени Институт Органической И Физической Химии Им.А.Е.Арбузова
Priority to SU1964276A priority Critical patent/SU475363A1/en
Application granted granted Critical
Publication of SU475363A1 publication Critical patent/SU475363A1/en

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Description

Пример 2. Тиоангидрид хлорциклогексллтритиофосфоновой кислоты.Example 2. Chlorocyclohexolltrithiophosphonic acid thioanhydride.

Через 10 г хлорциклогексилдихлорфосфина и 1,5 г элементарной серы при 130-140°С пропускают сухой сероводород в течеппе 3-5 час.After 10 g of chlorocyclohexyl dichlorophosphine and 1.5 g of elemental sulfur at 130-140 ° C, dry hydrogen sulfide is passed in a flow for 3-5 hours.

После перекрнсталлизацпп из хлорбензола получают 8,7 г (92%) белого кристаллического вендества; т. пл. 188-189°С.After cross-installing from chlorobenzene, 8.7 g (92%) of a white crystalline solid are obtained; m.p. 188-189 ° C.

Пайдеио, %: С1 16,57; Р 14,16; S 30,18.Paydeio,%: C1 16.57; R 14.16; S 30.18.

C,,H.,oCl2P2S4.C ,, H., oCl2P2S4.

Вычислено, %: С1 16,67; Р 14,56; S 30,15.Calculated,%: C1 16.67; R 14.56; S 30.15.

Пример 3. Тиоангидрид хлорциклогексилтритиофосфоновой кислоты.Example 3. Chlorocyclohexyltriothiophosphonic acid thioanhydride.

Через 6,4 г элемептариой серы, раствореиной в 50 мл абсолютного хлорбензола, при 132-135°С пропускают сухой сероводород (0,5 час). Затем :прн этой температуре к реакционной смесп нрн токе сероводорода прпкапывают 44 г хлорциклогексплднхлорфосфп1 а.After 6.4 g of sulfur elemeptaria, dissolved in 50 ml of absolute chlorobenzene, dry hydrogen sulfide is passed at 132-135 ° C (0.5 hour). Then: at this temperature, 44 g of chlorocyclohexpldnchlorophosphate 1 a is applied to the reaction mixture at this temperature of hydrogen sulfide.

После полного прибавлени  фосфина в реакцпоиную .маюсу при 135-140°С выдерживают 4 час. После охлаждени  кристаллы отфильтровывают и получают 38 г (89,1%) белого кристаллического вещества; т. пл. 188°С.After complete addition of phosphine to the reaction tank at 135-140 ° C, it is held for 4 hours. After cooling, the crystals are filtered off and 38 g (89.1%) of a white crystalline substance are obtained; m.p. 188 ° C.

Найдено, %: С1 16,60; Р 14,30; S 30,14.Found,%: C1 16.60; R 14.30; S 30.14.

Ci2H2oCl2P2S4Ci2H2oCl2P2S4

Вычислено, %: С1 16,67; Р 14,56; S 30,15.Calculated,%: C1 16.67; R 14.56; S 30.15.

Предмет изобретени Subject invention

Claims (2)

1. Способ получени  тноангидридов хлорциклоалкилтритиофосфоновых кислот на основе дихлорангидрида кислоты фосфора и сероводорода при нагреваниИ, отличающийс  тем, что, с целью упрощени  процесса и увеличеПИЯ выхода целевого продукта, дихлорангидрид хлорциклоалкилфосфопистой кислоты иодвергают взаимодействию с серой и сероводородом .1. A process for preparing tnoangidridov hlortsikloalkiltritiofosfonovyh acids based on phosphorus acid dichloride and hydrogen sulfide when heated, characterized in that, in order to simplify the process and the yield uvelichePIYa, hlortsikloalkilfosfopistoy acid dichloride iodvergayut reacted with sulfur and hydrogen sulfide. 2. Способ по п. 1, отличающийс  тем, что нагревание ведут до 100-200°С.2. A method according to claim 1, characterized in that the heating is carried out to 100-200 ° C.
SU1964276A 1973-10-03 1973-10-03 Method for producing chlorocycloalkyltriothiophosphonic acid thioanhydrides SU475363A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU1964276A SU475363A1 (en) 1973-10-03 1973-10-03 Method for producing chlorocycloalkyltriothiophosphonic acid thioanhydrides

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SU1964276A SU475363A1 (en) 1973-10-03 1973-10-03 Method for producing chlorocycloalkyltriothiophosphonic acid thioanhydrides

Publications (1)

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SU475363A1 true SU475363A1 (en) 1975-06-30

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109438708A (en) * 2018-10-10 2019-03-08 大连理工大学 A kind of preparation method of aliphatic poly monothioester

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109438708A (en) * 2018-10-10 2019-03-08 大连理工大学 A kind of preparation method of aliphatic poly monothioester
CN109438708B (en) * 2018-10-10 2020-11-03 大连理工大学 Preparation method of aliphatic polythioester

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