HRID1048731

反应详情

EQUATION

反应方程式

HRID 1048731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Sodium (9.3 g, 0.18 mol) was added to a degassed solution of 2-methyl-2-propanethiol (20.9 mL, 0.18 mol) in dry DMF (105 mL), under stirring at 0° C. in nitrogen atmosphere. The mixture was allowed to reach room temperature (RT, 20-25° C.) and stirred overnight. 1,2,4,5-Tetrachlorobenzene (8.0 g, 0.037 mol) was then added and the resulting mixture was stirred at RT for 2 h and then gently refluxed for 18 h. After cooling at RT, the reaction mixture was poured over ice (100 g), the precipitate was removed by filtration, washed with water, and dried to give 11.0 g of the title compound as an off-white powder.

WORKUP

后处理

  1. customto reach room temperature
  2. custom(RT, 20-25° C.)
  3. stirringstirred overnight
  4. stirringthe resulting mixture was stirred at RT for 2 h
  5. temperaturegently refluxed for 18 h
  6. temperatureAfter cooling at RT
  7. customthe precipitate was removed by filtration
  8. washwashed with water
  9. customdried