HRID133570
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe resulting reaction mixture
- stirringsubsequently stirred at 25° C. for 16 hours
- washwashed with water (30 mL×3)
- dry with materialThe organic layer was dried (over MgSO4)
- concentrationconcentrated
- customThe obtained crude product
- customwas purified by chromatography (SiO2, methanol-dichloromethane) to thereby provide 2-carbamoyl-1-(4-chlorobenzyl)pyrrolidine (5.21 g, 81%)