HRID584179

反应详情

EQUATION

反应方程式

HRID 584179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 3,5-dichlorobenzoic acid (2.6 g), (3R)-1-benzyl-3-(3,4-dimethylbenzyl)piperazine dihydrochloride (5.0 g) and triethylamine (8.54 ml) in dichloromethane (80 ml) was added 2-chloro-1-methylpyridinium iodide (3.83 g) under ice-cooling, and then the mixture was stirred at room temperature for 1 hour. The mixture was evaporated under reduced pressure, and the resulting residue was dissolved into ethyl acetate. The ethyl acetate solution was filtrated and evaporated under reduced pressure. The resulting residue was purified by column chromatography on silica gel using hexane-ethyl acetate (10:1) as eluent to give (2R)-4-benzyl-1-(3,5-dichlorobenzoyl)-2-(3,4-dimethylbenzyl)piperazine (5.58 g).

WORKUP

后处理

  1. temperaturecooling
  2. customThe mixture was evaporated under reduced pressure
  3. dissolutionthe resulting residue was dissolved into ethyl acetate
  4. filtrationThe ethyl acetate solution was filtrated
  5. customevaporated under reduced pressure
  6. customThe resulting residue was purified by column chromatography on silica gel