HRID1605385

反应详情

EQUATION

反应方程式

HRID 1605385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

184 G of 2-ethylcapronic acid allyl ester (prepared from the free acid and allyl alcohol by azeotropic esterification in benzene in the presence of p-toluenesulfonic acid; BP18 : 95°C; nD20 : 1.4298) was heated to 75°C in a 3-necked flask provided with stirrer, reflux condenser, internal thermometer and dropping funnel. Then 0.1 ml of an 0.01 molar solution of mesityl oxide-platinum dichloride catalyst complex in acetone was stirred in, and a quantity of 164 g of triethoxysilane was fed in from the dropping funnel within a 6-minute period, during which the temperature rose to 99°C. 10 minutes after the triethoxysilane feed was completed, no more silane hydrogen was analytically detectable. Vaccuum distillation of the product yielded 322 g of 3-(2'-ethylcaproyloxy)-propyltriethoxysilane, BP1 : 134°-138°C.

WORKUP

后处理

  1. custom95°C
  2. customprovided with stirrer
  3. temperaturereflux condenser
  4. waitwas fed in from the dropping funnel within a 6-minute period, during which
  5. customrose to 99°C
  6. custom10 minutes
  7. distillationVaccuum distillation of the product