SU233666A1 - - Google Patents
Info
- Publication number
- SU233666A1 SU233666A1 SU1193128A SU1193128A SU233666A1 SU 233666 A1 SU233666 A1 SU 233666A1 SU 1193128 A SU1193128 A SU 1193128A SU 1193128 A SU1193128 A SU 1193128A SU 233666 A1 SU233666 A1 SU 233666A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- styrene
- mol
- styrylphosphine
- heated
- mixture
- Prior art date
Links
- PPBRXRYQALVLMV-UHFFFAOYSA-N styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 3
- VZGDMQKNWNREIO-UHFFFAOYSA-N Carbon tetrachloride Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N methylene dichloride Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 2
- 241001344923 Aulorhynchidae Species 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N Phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000001264 neutralization Effects 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- -1 oxyl Chemical group 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
Description
СПОСОБ ПОЛУЧЕНИЯ ТРИ-р-СТИРИЛФОСФИНОКСИДЛMethod of producing tri-p-styrylphosphine oxyl
Изобретение относитс к способу получени три-р-стирилфосфиноксида(CeHjCH This invention relates to a process for the preparation of tri-p-styrylphosphine oxide (CeHjCH
СНз). SNS).
Это соединение может найти применение в качестве мономера дл получени отверждающихс негорючих композиций, в синтезе разнообразных фосфорорганических соединений.This compound can be used as a monomer for the preparation of curable, non-flammable compositions, in the synthesis of various organophosphorus compounds.
Предлагаемый способ основан на взаимодействии п тихлористого фосфора сначала с 2 моль стирола при нагревании до 80-90°С; затем еще с 1 моль стирола при нагревании до 130-140° с иоследующей обработкой смеси водой и выделением иродукта известным способом .The proposed method is based on the interaction of p-chloride of phosphorus first with 2 mol of styrene when heated to 80-90 ° C; then with another 1 mol of styrene when heated to 130-140 ° C, followed by treating the mixture with water and isolating the product in a known manner.
П р и м е р. Смесь 83,2 г (0,8 г моль стирола и 83,3 г (0,4 г моль) п тихлористого фосфора нагревают н иеремешивают 6 час при 80-90°С. Затем добавл ют 41,6 г (0,4 г моль) стирола и перемешивают 9 час при 130 - 140°С.PRI me R. A mixture of 83.2 g (0.8 g mol of styrene and 83.3 g (0.4 g mol) of phosphorus pentachloride is heated and stirred up for 6 hours at 80-90 ° C. Then 41.6 g (0.4 g mol) of styrene and stirred for 9 hours at 130 - 140 ° C.
К охлажденному до комнатной температуры продукту прибввл уот ири перемешивании 150 мл воды так, чтобы температура не иовышалась выше 40-50°С. Реакционную смесь довод т до сильно ш,елочной реакции. Осадок To the product cooled to room temperature, stir the mixture with 150 ml of water so that the temperature does not rise above 40-50 ° C. The reaction mixture is adjusted to a strongly wooded reaction. Sediment
отфильтровывают, иромывают водой до нейтральной реакции и сушат ири . Выход три-р-стирилфосфиноксида 34,5 г (24,2с/о). Дл очистки продукт перекристаллизовывают из водного спирта. Т. пл. возогнанного в вакууме препарата 241-242°С. Три-р-стирилфосфиноксид - бесцветный мелкокристаллический иорошок, растворимый в бензоле, хлороформе , хлористом метилене, спирте, не растворимый в воде, петролейном эфире, четырсххлористом углероде.filtered, tromp with water until neutral, and dried irie. The output of the three-p-styrylphosphine oxide 34,5 g (24,2s / o). The product is recrystallized from aqueous alcohol for purification. T. pl. vacuum-boosted preparation 241-242 ° С. Three-p-styrylphosphine oxide is a colorless crystalline powder and soluble in benzene, chloroform, methylene chloride, alcohol, insoluble in water, petroleum ether, carbon tetrachloride.
Пайдено, %: С 81,14; 81.27: П 6.08; 5,91; Р 8,21; 8,47.Paydeno,%: C 81.14; 81.27: P 6.08; 5.91; P 8.21; 8.47.
CisHoiOP.CisHoiOP.
Вычислено, Vc: С 80,88; Н 5,94; Р 8,69.Calculated Vc: C, 80.88; H 5.94; P 8,69.
Предмет изобретени Subject invention
Способ получени три-р-стирилфосфиноксида , отличающийс тем, что и тихлорист1з1Й фосфор подвергают взаимодействию с 2 лголб стирола при нагревании до 80-90°С и добавл ют к реакционной массе еще 1 моль стирола при нагревании до 130-140°С с последующей обработкой смеси водой и выделением продукта известным способом.A process for preparing tri-p-styrylphosphine oxide, characterized in that phosphorous also phosphorus is reacted with 2 lg of styrene when heated to 80-90 ° C and another 1 mol of styrene is added to the reaction mass when heated to 130-140 ° C with subsequent processing mixture with water and isolation of the product in a known manner.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU233666A1 true SU233666A1 (en) |
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