HRID584175

反应详情

EQUATION

反应方程式

HRID 584175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2R)-4-benzyl-1-(3,5-dichlorobenzoyl)-2-(3,4-dimethylbenzyl)piperazine (5.03 g) in dichloromethane (50 ml) was added 1-chloroethyl chloroformate (1.51 ml) slowly at 0° C., and then the mixture was heated at reflux under stirring. After 5.5 hours, the solvent was removed in vacuo and then the resulting residue was dissolved in methanol (20 ml) and refluxed for 0.5 hour. After removal of the solvent, the resulting residue was triturated with isopropyl ether to afford (2R)-1(3,5-dichlorobenzoyl)-2-(3,4-dimethylbenzyl)piperazine hydrochloride (4.84 g).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux
  3. customthe solvent was removed in vacuo
  4. dissolutionthe resulting residue was dissolved in methanol (20 ml)
  5. temperaturerefluxed for 0.5 hour
  6. customAfter removal of the solvent
  7. customthe resulting residue was triturated with isopropyl ether