HRID615435

反应详情

EQUATION

反应方程式

HRID 615435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a reaction vessel fitted with a magnetic stirrer, 2.31 grams (10 mmole) of 2-chloro-6-(trichloromethyl)pyridine was dissolved in 25 ml of N-methylpyrrolidone. To this mixture was added 2.0 grams of 50% aqueous sodium hydroxide and 1.29 grams (10.2 mmole) of dimethyl phosphite. Within five minutes the temperature rose from 24° C. to 55° C. Analysis by glc indicated a ratio of 97.6/1.7 for reduced product to starting material. The reaction mixture was poured into 100 ml of water and the oil which separated was crystallized to form 1.4 grams of 2-chloro-6-(dichloromethyl)pyridine (mp 50°-53° C.). The yield was calculated to be 71% of theoretical.

WORKUP

后处理

  1. customIn a reaction vessel fitted with a magnetic stirrer
  2. customthe oil which separated
  3. customwas crystallized