HRID2047439

反应详情

EQUATION

反应方程式

HRID 2047439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of the compound (33.4 g) obtained in step 2 in acetonitrile (250 mL) was added ACE-Cl (13.9 g) at room temperature, and the mixture was stirred at 90° C. for 2 hr. The reaction solution was cooled, and the solvent was evaporated under reduced pressure. To the residue was added methanol (250 mL), and the mixture was stirred at 80° C. for 2 hr. The reaction solution was cooled, the solvent was evaporated under reduced pressure, and the residue was washed with ethyl acetate/IPE to give methyl (3R*,4S*)-4-(3,4-dichlorophenyl)pyrrolidine-3-carboxylate monohydrochloride (26.9 g, 98%) as a pale-yellow powder.

WORKUP

后处理

  1. temperatureThe reaction solution was cooled
  2. customthe solvent was evaporated under reduced pressure
  3. additionTo the residue was added methanol (250 mL)
  4. stirringthe mixture was stirred at 80° C. for 2 hr
  5. temperatureThe reaction solution was cooled
  6. customthe solvent was evaporated under reduced pressure
  7. washthe residue was washed with ethyl acetate/IPE