HRID133570

反应详情

EQUATION

反应方程式

HRID 133570 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Triethylamine (7.45 mL) and 4-chlorobenzyl chloride (3.88 g, 24.1 mmol) were added to an acetonitrile (35 mL) solution of dl-prolinamide hydrochloride (2.5 g, 21.8 mmol). The resulting reaction mixture was stirred at 70° C. for 4 hours and subsequently stirred at 25° C. for 16 hours. The resulting mixture was diluted with dichloromethane (20 mL) and washed with water (30 mL×3). The organic layer was dried (over MgSO4) and concentrated. The obtained crude product was purified by chromatography (SiO2, methanol-dichloromethane) to thereby provide 2-carbamoyl-1-(4-chlorobenzyl)pyrrolidine (5.21 g, 81%).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. stirringsubsequently stirred at 25° C. for 16 hours
  3. washwashed with water (30 mL×3)
  4. dry with materialThe organic layer was dried (over MgSO4)
  5. concentrationconcentrated
  6. customThe obtained crude product
  7. customwas purified by chromatography (SiO2, methanol-dichloromethane) to thereby provide 2-carbamoyl-1-(4-chlorobenzyl)pyrrolidine (5.21 g, 81%)