HRID1679061

反应详情

EQUATION

反应方程式

HRID 1679061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.4 g. of 5-chloro-2-(2-hydroxyethyl)-3-phenylisoindole-1-carboxylic acid ethyl ester and 3.4 ml. of triethylamine in 60 ml. of methylene chloride is treated dropwise at 15°-20° C. with 1.6 ml. of methane sulfochloride. The mixture is subsequently left standing for 30 minutes at room temperature, then diluted with methylene chloride to three times the volume. The solution is washed successively with water, 0.5-N hydrochloric acid, 5% sodium bicarbonate solution and again with water. After drying over sodium sulfate and evaporation of the solution, there is obtained 5-chloro-2-{2-[(methylsulfonyl)oxy]ethyl}-3-phenylisoindole-1-carboxylic acid ethyl ester; melting point 125°-127° C. Recrystallization from methylene chloride/hexane does not increase the melting point.

WORKUP

后处理

  1. waitThe mixture is subsequently left
  2. washThe solution is washed successively with water, 0.5-N hydrochloric acid, 5% sodium bicarbonate solution and again with water
  3. dry with materialAfter drying over sodium sulfate and evaporation of the solution