HRID2412305

反应详情

EQUATION

反应方程式

HRID 2412305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The sodium salt of 4-chloro-3-[(2,2-dichlorocyclopropyl)methoxy]phenol as prepared from 20 g of 4-chloro-3-[(2,2-dichlorocyclopropyl)methoxy]phenol and 16 g of a 28% methanol solution of sodium methylate was dissolved in 300 ml of water and the solution was added dropwise to a solution of 5 ml of trichloromethyl chloroformate in 100 ml of chloroform while maintaining the reaction temperature at 10° C. or below. The reaction mixture was allowed to stand for phase separation. The chloroform layer was dried over anhydrous magnesium sulfate and the solvent was then distilled off. There was obtained 22.5 g of 4-chloro-3-[(2,2-dichlorocyclopropyl)methoxy]phenyl chloroformate.

WORKUP

后处理

  1. temperaturewhile maintaining the reaction temperature at 10° C. or below
  2. customto stand for phase separation
  3. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was then distilled off