SU498311A1 - Method for preparing bis- (perfluoroalkyl) phosphinic acid - Google Patents

Method for preparing bis- (perfluoroalkyl) phosphinic acid

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Publication number
SU498311A1
SU498311A1 SU1883723A SU1883723A SU498311A1 SU 498311 A1 SU498311 A1 SU 498311A1 SU 1883723 A SU1883723 A SU 1883723A SU 1883723 A SU1883723 A SU 1883723A SU 498311 A1 SU498311 A1 SU 498311A1
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SU
USSR - Soviet Union
Prior art keywords
perfluoroalkyl
phosphinic acid
preparing bis
bis
calculated
Prior art date
Application number
SU1883723A
Other languages
Russian (ru)
Inventor
Валерий Яковлевич Семений
Владимир Николаевич Завацкий
Николай Иванович Липтуга
Лев Моисеевич ЯГУПОЛЬСКИЙ
Original Assignee
Институт Органической Химии Ан Усср
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Application filed by Институт Органической Химии Ан Усср filed Critical Институт Органической Химии Ан Усср
Priority to SU1883723A priority Critical patent/SU498311A1/en
Application granted granted Critical
Publication of SU498311A1 publication Critical patent/SU498311A1/en

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Description

Найдено, %: С 17,76; 17,86; Н 0,47; 0,51; Р 7,40; 7,60. СбНРиОгР. Вычислено, %: С 17,93; Н 0,25; Р 7,71. Аналогично получают 6uc-(Rf - фосфиновые кислоты, неречисленные в таблице. Пример 2. В круглодонную колбу на 25 мл, снабженную обратным холодильником, помещают 14,5 г (0,017 г-моль трис-(Еерфторизоамил )-фосфииоксида и 1,0 г (0,055 г-моль) воды и нагревают от 100 до 150° С в течение 3 час. Летучие иродукты улавливают в системе ловушек (-70° С). После охлаждени  реакционной массы неотогнанные летучие продукты отсасывают в вакууме в течение 1.0 мин в систему ловушек. Потер  в весе 4,8 г (отш,енление одного изо-СбРп соответствует потере в весе 4,6 г). Полученный изо-СбРцН идентифицируют повторной перегонкой, т. кип. 38-41° С. К полученной водной кислоте прибавл ют 3,5 г (0,03 г-моль) хлористого тионила, кип т т до прекрашени  выделени  газа (1 час), отгон ют избыток хлористого тионила, перегон ют остаток в вакууме и получают 8,7 г (85,0%) быс-(перфторизоамил) - фосфиновой кислоты, бесцветные гигроскопичные на воздухе кристаллы, т. пл. 49-5Г С. Найдено, %: С 19,43; 19,60; Н 0,25; 0,34; Р 5,51; 5,67. CioHFssOP. Вычислено, %: С 19,97; Н 0,17; Р 5,15. В аналогичных услови х получают бис (Нр)-фосфиновые кислоты, указанные в той же таблице.Found,%: C 17.76; 17.86; H 0.47; 0.51; P 7.40; 7.60. SbNrOiGR. Calculated,%: C 17.93; H 0.25; R 7.71. Similarly, 6uc- (Rf-phosphinic acids not listed in Table 1 are prepared. Example 2. In a 25 ml round-bottom flask equipped with a reflux condenser, 14.5 g (0.017 g-mol of tris- (Eurfluoroisoamyl) phosphosioxide and 1.0 g (0.055 g-mol) of water and heated from 100 to 150 ° C for 3 hours. The volatiles and products are trapped in the trap system (-70 ° C). After cooling the reaction mass, the non-distilled volatile products are sucked off in a vacuum system for 1.0 min. Loss in weight of 4.8 g (otsh, enenie one Iso-SbRp corresponds to a loss in weight of 4.6 g.) Received izo-SbRtsN id Identified by re-distillation, bp 38-41 ° C. To the resulting aqueous acid was added 3.5 g (0.03 g-mol) of thionyl chloride, boiled until the evolution of gas ceased (1 hour), the excess thionyl chloride, the residue is distilled in vacuum and 8.7 g (85.0%) of bys- (perfluoroisoamyl) -phosphinic acid are obtained, colorless crystals hygroscopic in air, mp 49-5 ° C. Found: C 19 , 43; 19.60; H: 0.25; 0.34; P 5.51; 5.67. CioHFssOP. Calculated,%: C 19.97; H 0.17; P 5.15. Under similar conditions, bis (Hp) -phosphonic acids are obtained, indicated in the same table.

Claims (1)

5 1,3092; Й4 1,800; ЛШп32,25 (вычислено 32,12). Формула изобретени  Способ получени  бис-(перфторалкил)фосфиновых кислот гидролизом трис- (перс| )торалкил)-фосфиноксидов водной, отличающийс  тем, что, с целью упрощени  способа, процесс провод т при 100-150°С с последующем выделением целевого продукта при кип чении полученной омеси с хлористым тионилом.5 1.3092; H4 1,800; LSh32.25 (calculated 32.12). The method of obtaining bis- (perfluoroalkyl) phosphinic acids by hydrolysis of tris (pers |) toralkyl) phosphine oxides with water, characterized in that, in order to simplify the process, the process is carried out at 100-150 ° C, followed by isolation of the desired product at boiling omesy with thionyl chloride.
SU1883723A 1973-02-16 1973-02-16 Method for preparing bis- (perfluoroalkyl) phosphinic acid SU498311A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU1883723A SU498311A1 (en) 1973-02-16 1973-02-16 Method for preparing bis- (perfluoroalkyl) phosphinic acid

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Application Number Priority Date Filing Date Title
SU1883723A SU498311A1 (en) 1973-02-16 1973-02-16 Method for preparing bis- (perfluoroalkyl) phosphinic acid

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SU498311A1 true SU498311A1 (en) 1976-01-05

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7202379B2 (en) 2002-04-16 2007-04-10 Merck Patent Gmbh Process for the preparation of bis(perfluoroalkyl)phosphinic acids and salts thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7202379B2 (en) 2002-04-16 2007-04-10 Merck Patent Gmbh Process for the preparation of bis(perfluoroalkyl)phosphinic acids and salts thereof

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