HRID250737

反应详情

EQUATION

反应方程式

HRID 250737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Combine 2-iminopyrrolidine hydrochloride (6.98 g, 57.8 mmol) (Callahan, et al., J. Med. Chem. 45, 999-1001 (2002)), 2-bromoacetophenone (3.8 g, 19.3 mmol), and sodium carbonate (8.2 g, 77.2 mmol) in dry dimethylformamide (25 mL). Heat at 80° C. for 18 hours. Cool to room temperature, add water (60 mL), and extract with ethyl acetate (3×100 mL). Concentrate the combined organic layers under reduced pressure. Dilute the residue with diethyl ether (100 mL), wash with cold water (3×80 mL), and concentrate under reduced pressure to provide the desired compound as a white solid (3.2 g, 89%).

WORKUP

后处理

  1. temperatureCool to room temperature
  2. extractionextract with ethyl acetate (3×100 mL)
  3. concentrationConcentrate the combined organic layers under reduced pressure
  4. additionDilute the residue with diethyl ether (100 mL)
  5. washwash with cold water (3×80 mL)
  6. concentrationconcentrate under reduced pressure