HRID1606845

反应详情

EQUATION

反应方程式

HRID 1606845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

107 g (1 mol) of the ammonium salt of α-fluoroacrylic acid are mixed with 14.5 g (0.2 mol) of dimethylformamide and 0.6 liter of xylene, and 131 g (1.1 mol) of thionyl chloride are added dropwise to the mixture in the course of one hour; the mixture is then warmed at a temperature of 80° C. for two hours. After cooling to a temperature of 0° C., a mixture of 204 g (1.1 mol) of tributylamine and 185 g (1.1 mol) of hexafluoroisopropanol is added to the reaction mixture in the course of 30 minutes. The mixture is then stirred at a temperature of 30° C. for a further hour and is finally filtered. The filtrate is distilled under a pressure of 270 mbar and hexafluoroisopropyl α-fluoroacrylate is obtained as a colorless liquid.

WORKUP

后处理

  1. additionare added dropwise to the mixture in the course of one hour
  2. temperatureAfter cooling to a temperature of 0° C.
  3. additionis added to the reaction mixture in the course of 30 minutes
  4. filtrationis finally filtered
  5. distillationThe filtrate is distilled under a pressure of 270 mbar