HRID1260922

反应详情

EQUATION

反应方程式

HRID 1260922 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 mixture was cooled, and the solvent was evaporated under reduced pressure. Methanol (250 mL) was added to the residue, and the mixture was stirred at 80° C. for 2 hr. The reaction mixture was cooled, and the solvent was evaporated under reduced pressure 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 mixture was cooled
  2. customthe solvent was evaporated under reduced pressure
  3. additionMethanol (250 mL) was added to the residue
  4. stirringthe mixture was stirred at 80° C. for 2 hr
  5. temperatureThe reaction mixture was cooled
  6. customthe solvent was evaporated under reduced pressure