HRID2380085

反应详情

EQUATION

反应方程式

HRID 2380085 的结构方程式

PROCEDURE

实验过程

To a mixture of 200 g (0.667 mol) of 2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethylamine, 81 g (0.80 mol) of triethylamine and 8 liter of toluene, there was added dropwise a solution of 70 g (0.67 mol) of cyclopropane carbonylchloride in 2 liter of toluene with stirring at a temperature of from 5° C. to 10° C. After 2 hours, the reaction mixture was stirred at a room temperature for 15 hours. After the reaction was completed, the resultant mixture was washed twice with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 163 g of N-{2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethyl}-cyclopropane carboxyamide as a white crystal (m.p. 89°-90° C.).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred at a room temperature for 15 hours
  2. washthe resultant mixture was washed twice with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure