HRID442051

反应详情

EQUATION

反应方程式

HRID 442051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

About 468 grams (4.5 moles) of styrene and about 0.5 grams of di-t-butyl-p-cresol were charged to a one liter, three necked round bottom flask fitted with a magnetic stirrer, thermometer, dropping funnel and reflux condenser bearing a nitrogen by-pass on the vent. While stirring the flask contents were heated to 90° C, and a sufficient amount of about a 2% solution of chloroplatinic acid catalyst dissolved in dimethylether of ethylene glycok to give about 25 parts by weight of plantinum per million parts by weight of reactants was added. Then about 610 grams (4.5 moles) of trichlorosilane were slowly and continuously added via the dropping funnel over a one and one-half hour period while maintaining the reaction temperature at 90°-95° C. A vapor phase chromatogram on the reaction contents indicated there was an essentially complete conversion to product. The crude silane reaction product was then refined by a one plate distillation at 0.1 mm. pressure to yield about 1015 grams (4.24 moles) of phenylethyltrichlorosilane product ##STR22## (94.5% conversion) which had a boiling point of about 63°-64° C./0.1 mm Hg.

WORKUP

后处理

  1. customfitted with a magnetic stirrer
  2. temperaturereflux condenser
  3. customto give about 25 parts by weight of plantinum per million parts by weight of reactants
  4. additionwas added
  5. additioncontinuously added via the dropping funnel over a one and one-half hour period
  6. temperaturewhile maintaining the reaction temperature at 90°-95° C
  7. customA vapor phase chromatogram on the reaction contents
  8. distillationwas then refined by a one plate distillation at 0.1 mm