HRID2047439
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
- 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
- temperatureThe reaction solution was cooled
- customthe solvent was evaporated under reduced pressure
- additionTo the residue was added methanol (250 mL)
- stirringthe mixture was stirred at 80° C. for 2 hr
- temperatureThe reaction solution was cooled
- customthe solvent was evaporated under reduced pressure
- washthe residue was washed with ethyl acetate/IPE