HRID847476

反应详情

EQUATION

反应方程式

HRID 847476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

In a 1 liter four-neck flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer were placed 108.5 g (1.0 mol) of trimethylchlorosilane, 111.1 g (1.1 mol) of triethylamine and 300 ml of hexane. Thereto, 73.0 g (1.0 mol) of diethylamine was added dropwise from the dropping funnel over a 1-hour period. During the addition, the temperature of the reaction system was kept within the range of 20° C. to 60° C. to make the reaction be proceeding. At the conclusion of the addition, the temperature was raised to 50-60° C. and kept there for 2 hours, whereby the reaction was matured. Then, the reaction mixture was filtered through a glass filter to remove the salt yielded as a by-product. The filtrate was allowed to stand for one day at room temperature to precipitate the salt. The salt precipitated was filtered off, and the filtrate was subjected to distillation under ordinary pressure to obtain 136.3 g of diethylaminotrimethylsilane as a fraction having a boiling point of 125-126° C. The yield was 94%, and the chlorine concentration was 146 ppm.

WORKUP

后处理

  1. customIn a 1 liter four-neck flask equipped with a stirrer, a reflux condenser, a dropping funnel
  2. additionDuring the addition
  3. customwas kept within the range of 20° C. to 60° C.
  4. additionAt the conclusion of the addition
  5. filtrationThen, the reaction mixture was filtered through a glass
  6. filtrationfilter
  7. customto remove the salt
  8. customyielded as a by-product
  9. waitto stand for one day at room temperature
  10. customto precipitate the salt
  11. customThe salt precipitated
  12. filtrationwas filtered off
  13. distillationthe filtrate was subjected to distillation under ordinary pressure