HRID26688

反应详情

EQUATION

反应方程式

HRID 26688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
171 °C

PROCEDURE

实验过程

A suspension of 22.7 g of sodium p-toluenesulphinate in 50 ml of dimethyl methanephosphonate is treated with 12.6 g of triethylamine and the mixture is heated in the course of 45 minutes to 167° C. The temperature is raised further to 171° C. and kept thereat for a further 30 minutes. The cooled solution is poured into 700 ml of water and stired for 1 hour. The precipitated crystalline product is collected by filtration and washed with 350 ml of water. The residue is dried at 25 torr and 50° C., affording 17.2 g (80.9% of theory) of p-tolylmethylsulphone of the formula ##STR14## with a melting point of 85°-96° C. and a purity of 95.8%.

WORKUP

后处理

  1. temperaturethe mixture is heated in the course of 45 minutes to 167° C
  2. waitstired for 1 hour
  3. filtrationThe precipitated crystalline product is collected by filtration
  4. washwashed with 350 ml of water
  5. customThe residue is dried at 25 torr and 50° C.