HRID5224

反应详情

EQUATION

反应方程式

HRID 5224 的结构方程式

CONDITIONS

反应条件

温度
93 °C

PROCEDURE

实验过程

150 g of solid 1,1-bis(chlorophenyl)-2,2,2-trichloroethane were added to 248.8 g of a 27.2% strength aqueous sodium hydroxide solution maintained at 93° C. 1.4 g of dimethyllaurylbenzylammonium chloride were added thereto. The temperature increased from 93° to 103° C. The addition of solid 1,1-bis(chlorophenyl)-2,2,2-trichloroethane was continued up to a total amount of 300 g. 1.1 g of dimethyllaurylbenzylammonium chloride were added again and the temperature was maintained between 100° and 105° C. for 14 hours, 30 min. The organic phase was separated off by phase separation and washed three times with 100 g of a 1N solution of sulfuric acid and with water (100 g). 263.7 g of 1,1-bis(chlorophenyl)-2,2-dichloroethylene were obtained (y=98.0%) with 0.09% of 1,1-bis(chlorophenyl)-2,2,2-trichloroethane.

WORKUP

后处理

  1. temperatureThe temperature increased from 93° to 103° C
  2. temperaturethe temperature was maintained between 100° and 105° C. for 14 hours, 30 min
  3. customThe organic phase was separated off by phase separation
  4. washwashed three times with 100 g of a 1N solution of sulfuric acid