HRID1373119

反应详情

EQUATION

反应方程式

HRID 1373119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.3 g (8.4 mmol) of 4-(N-aminocarbonylmethyl-N-methylsulphonyl-amino)-nitrobenzene are refluxed in 35 ml (35 mmol) of borane-THF (1 M solution in THF) 7 hours. Then 30 ml of 6 N hydrochloric acid are added, and the mixture is refluxed for another 8 hours. The solvent is distilled off, the residue is mixed with water and extracted with ethyl acetate. The aqueous phase is made alkaline with potassium carbonate and extracted with dichloromethane. The organic phase is separated off, dried and evaporated down.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for another 8 hours
  2. distillationThe solvent is distilled off
  3. additionthe residue is mixed with water
  4. extractionextracted with ethyl acetate
  5. extractionextracted with dichloromethane
  6. customThe organic phase is separated off
  7. customdried
  8. customevaporated down