HRID1679474

反应详情

EQUATION

反应方程式

HRID 1679474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.5 Kg. of 1-amino-2-nitro-5-phenylthiobenzene in 60 l. of methanol and 30 l. of water is treated, under nitrogen, with 8.0 kg. of sodium dithionite and 2.0 kg. of sodium carbonate at reflux. The mixture is heated for 2 hours and the methanol is removed by distillation. The mixture is cooled and extracted with dichloromethane. The dichloromethane solution is filtered, dried over sodium sulfate, and 1,2-diamino-4-phenylthiobenzene is isolated by evaporation.

WORKUP

后处理

  1. temperatureThe mixture is heated for 2 hours
  2. customthe methanol is removed by distillation
  3. temperatureThe mixture is cooled
  4. extractionextracted with dichloromethane
  5. filtrationThe dichloromethane solution is filtered
  6. dry with materialdried over sodium sulfate