SU498311A1 - Method for preparing bis- (perfluoroalkyl) phosphinic acid - Google Patents
Method for preparing bis- (perfluoroalkyl) phosphinic acidInfo
- 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
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- perfluoroalkyl
- phosphinic acid
- preparing bis
- bis
- calculated
- Prior art date
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- Compositions Of Macromolecular Compounds (AREA)
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)
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 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU1883723A SU498311A1 (en) | 1973-02-16 | 1973-02-16 | Method for preparing bis- (perfluoroalkyl) phosphinic acid |
Publications (1)
Publication Number | Publication Date |
---|---|
SU498311A1 true SU498311A1 (en) | 1976-01-05 |
Family
ID=20542699
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU1883723A SU498311A1 (en) | 1973-02-16 | 1973-02-16 | Method for preparing bis- (perfluoroalkyl) phosphinic acid |
Country Status (1)
Country | Link |
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SU (1) | SU498311A1 (en) |
Cited By (1)
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 |
-
1973
- 1973-02-16 SU SU1883723A patent/SU498311A1/en active
Cited By (1)
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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