HRID892629

反应详情

EQUATION

反应方程式

HRID 892629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(p-chlorophenyl)glycine (37.1 g, 0.2 mol) in methanol is treated with triethylamine (20.2 g, 0.2 mol), stirred for 10 minutes, treated dropwise with ethyl trifluoroacetate (35.5 g, 0.25 mol), stirred for 4 days, diluted with methanol and treated with Dowex 50×8-100 ion exchange resin. The reaction mixture is stirred for 10 minutes and filtered. The filter cake is washed with methanol. The filtrates are combined and concentrated in vacuo to afford a yellow solid which is recrystallized from 1,2-dichloroethane to give the title compound as white crystals, 26.4 g (46.8% yield), mp 170-172° C.

WORKUP

后处理

  1. stirringstirred for 4 days
  2. additiontreated with Dowex 50×8-100 ion exchange resin
  3. stirringThe reaction mixture is stirred for 10 minutes
  4. filtrationfiltered
  5. washThe filter cake is washed with methanol
  6. concentrationconcentrated in vacuo
  7. customto afford a yellow solid which
  8. customis recrystallized from 1,2-dichloroethane