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
PROCEDURE
实验过程
(3S,4R)-1-Benzyl-3-cyclopropylaminomethyl-4-methylpyrrolidine (25.0 g) was dissolved in ethanol (200 mL). To this solution, trifluoroacetic acid (15.7 mL) and 10% palladium carbon (12.5 g) were added and the mixture was stirred at room temperature for 9 hours under a hydrogen pressure of 3.9×105 Pa. The catalyst was collected from the reaction mixture by filtration and was washed with ethanol containing 25% water (300 mL). The filtrate and the washing solution were combined and the combined solution was concentrated under reduced pressure. The resultant pale brown crystal was suspended in tetrahydrofuran (100 mL) and was collected by filtration. The collected crystal was washed with tetrahydrofuran and was dried under reduced pressure to give 34.1 g of (3R,4R)-3-cyclopropylaminomethyl-4-methylpyrrolidine-trifluoroacetate as a white crystal.
WORKUP
后处理
- filtrationThe catalyst was collected from the reaction mixture by filtration
- washwas washed with ethanol containing 25% water (300 mL)
- concentrationthe combined solution was concentrated under reduced pressure
- filtrationwas collected by filtration
- washThe collected crystal was washed with tetrahydrofuran
- customwas dried under reduced pressure