反应详情

温度

60 °C

K2CO3 (3.02 g) and 4-chlorobenzyl chloride (3.52 g, 21.8 mmol) were successively added to an acetonitrile (100 mL) solution of 4-(aminomethyl)piperidine (7.00 g, 61.3 mmol). The resulting reaction mixture was stirred at 60° C. for 16 hours, cooled to 25° C. and concentrated. The obtained residue was fractionated between dichloromethane (75 mL) and water (50 mL) and then washed with water (50 mL×2) and brine (50 mL×1). The organic layer was dried (over MgSO4), concentrated and then purified by chromatography (SiO2, 4% H2O-iPrOH) to provide 4-(aminomethyl)-1-(4-chlorobenzyl)piperidine (3.58 g, 69%).

1. customThe resulting reaction mixture
2. temperaturecooled to 25° C.
3. concentrationconcentrated
4. washwashed with water (50 mL×2) and brine (50 mL×1)
5. dry with materialThe organic layer was dried (over MgSO4)
6. concentrationconcentrated
7. custompurified by chromatography (SiO2, 4% H2O-iPrOH)