HRID584175
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureat reflux
- customthe solvent was removed in vacuo
- dissolutionthe resulting residue was dissolved in methanol (20 ml)
- temperaturerefluxed for 0.5 hour
- customAfter removal of the solvent
- customthe resulting residue was triturated with isopropyl ether