HRID1295872
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
To a solution of chlorodiphenylmethane (0.79 g, 3.22 mmol) in butanone (20 ml) was added methyl-pyrrolidine-3-ylmethyl-amine)-carbamic acid tert-butyl ester (0.69 g, 3.22 mmol), K2CO3 (0.54 g, 3.8 mmol) and KI (0.54 g, 3.22 mmol). The mixture was heated under reflux for 18 hours, then filtered and the solvent was removed in vacuo. The residue was dissolved in CH2Cl2 (50 ml) and washed with water (10 ml). Drying over MgSO4 and removal of solvent under reduced pressure followed by column chromatography using CH2Cl2:CH3OH (20:1) gives the desired product in 75% yield.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 18 hours
- filtrationfiltered
- customthe solvent was removed in vacuo
- dissolutionThe residue was dissolved in CH2Cl2 (50 ml)
- washwashed with water (10 ml)
- dry with materialDrying over MgSO4 and removal of solvent under reduced pressure