HRID127002

反应详情

EQUATION

反应方程式

HRID 127002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 250 ml three-necked flask equipped with magnetic stirrer, reflux condenser and dropping funnel, 26.6 g of pentachlorophenol is placed for dissolving in 70 ml of chloroform and 50 ml of triethylamine. Over a period of 10 minutes, 22.1 g of 3-aminopropyltriethoxysilane is added, drop by drop, with refluxing and stirring. After three hours of boiling and stirring, the clear solution is concentrated by distilling out the chloroform, the ethanol that is formed, and most of the triethylamine, and the product is carefully precipitated with 130 ml of pentane, with stirring. It is washed thrice with pentane and decanted, then dried in a high vacuum at about 60° C. 41 g of a finely divided 3-aminopropyldiethoxypentachlorophenoxysilane is obtained having a melting point of 122° C.

WORKUP

后处理

  1. customIn a 250 ml three-necked flask equipped with magnetic stirrer
  2. temperaturereflux condenser
  3. temperaturedrop by drop, with refluxing
  4. waitAfter three hours of boiling
  5. stirringstirring
  6. concentrationthe clear solution is concentrated
  7. distillationby distilling out the chloroform
  8. customthe ethanol that is formed
  9. custommost of the triethylamine, and the product is carefully precipitated with 130 ml of pentane
  10. stirringwith stirring
  11. washIt is washed thrice with pentane
  12. customdecanted
  13. customdried in a high vacuum at about 60° C