SU232973A1 - METHOD OF OBTAINING CHLORANGIDRID DI - (^ hygrylphosphinic acid - Google Patents
METHOD OF OBTAINING CHLORANGIDRID DI - (^ hygrylphosphinic acidInfo
- Publication number
- SU232973A1 SU232973A1 SU1193688A SU1193688A SU232973A1 SU 232973 A1 SU232973 A1 SU 232973A1 SU 1193688 A SU1193688 A SU 1193688A SU 1193688 A SU1193688 A SU 1193688A SU 232973 A1 SU232973 A1 SU 232973A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- obtaining
- hygrylphosphinic
- chlorangidrid
- acid
- styrene
- Prior art date
Links
- 239000002253 acid Substances 0.000 title description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 5
- UHZYTMXLRWXGPK-UHFFFAOYSA-N Phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 claims description 3
- FAIAAWCVCHQXDN-UHFFFAOYSA-N Phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- -1 di-styrylphosphinic acid chloride Chemical compound 0.000 claims 1
- 238000002955 isolation Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 description 3
- HCSDJECSMANTCX-UHFFFAOYSA-N dichloro(methoxy)phosphane Chemical compound COP(Cl)Cl HCSDJECSMANTCX-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
изобретение касаетс области получени хлорангидрида ди-р-стирилфосфинистой кислоты , который может н-айтк применение в синтезе разнообразных фосфорорганических соединений.The invention concerns the field of production of di-p-styrylphosphinic acid chloride, which can be used in the synthesis of various organophosphorus compounds.
Предлагаемый способ основан на взаимодействии п тихлористого фосфора со стиролом при пагревании до 80-90С с последующим добавлением метилдихлорфосфита при нагревании до 65-70°С в среде треххлористого фосфора в качестве растворител .The proposed method is based on the interaction of phosphorus pentachloride with styrene when melting to 80-90 ° C, followed by the addition of methyldichlorophosphite when heated to 65-70 ° C in phosphorus trichloride as a solvent.
При;мер. Смесь 83,3 г (0,8 г-моль} стирола и 83,3 г (0,4 г моль) п тихлористого фосфора нагревают При 80-90°С и перемешивании 8 час, затем добавл ют 200 мл треххлористого фосфора н к образовавшейс суспензии прибавл ют по капл м и перемешивании при темнературе 65-70°С 53,2 г (0,4 г-моль) метилдихлорфосфита, перемешивание и нагревание продолжают до полной гомогенизации реакционной смеси. Растворитель н легколетучие продукты реакции отгоН ют Б вакууме водоструйного насоса. Перегонкой остатка выдел ют 47 г (43%) хлорапгидрида ди-р-стирилхлорфосфинистой кнс.тоты с т. кип. 229-231°С (0,06 мм рт. ст.) в виде очень в зкой прозрачной массы, .медленно кристаллизующейс при хранении.Example. A mixture of 83.3 g (0.8 g-mol} styrene and 83.3 g (0.4 g mol) of phosphorus pentachloride is heated at 80-90 ° C and stirring for 8 hours, then 200 ml of phosphorus trichloride are added to the resulting suspension is added dropwise and stirring at a temperature of 65-70 ° C with 53.2 g (0.4 g-mol) of methyldichlorophosphite, stirring and heating are continued until the reaction mixture is completely homogenized.The solvent and volatile reaction products are distilled off In a water jet vacuum pump. Distillation of the residue yields 47 g (43%) of chloroaphyde di-p-styrylchlorophosphine sulphate with Kip. 229-231 ° C (0.06 mm Hg) as a very viscous, transparent mass that slowly crystallizes during storage.
Найдено, %: Р 10,93; 11,03; С1 13,00; 13,04.Found,%: P 10.93; 11.03; C1 13.00; 13.04.
CioHuClP. CioHuClP.
,: Р 10,99; С1 13,01. Вычислено,: P 10.99; C1 13.01. Calculated
10ten
Предмет изобретени Subject invention
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU232973A1 true SU232973A1 (en) |
Family
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