反应详情

温度

70 °C

p-Chlorobenzyl chloride (463 mg, 2.9 mmol) and K2CO3 (828 g, 6 mmol) were added to an acetonitrile (45 mL) solution of 3-aminohomopiperidine (1.71 g, 15 mmol), and the resulting mixture was stirred at 70° C. with heating for 9 hours, cooled to 25° C. and concentrated to afford a yellow solid. The resulting residue was partitioned between H2O (5 mL) and ethyl acetate (50 mL) and the aqueous layer was extracted with ethyl acetate (50 mL×2). The organic layers were combined, washed with brine (20 mL), dried (over MgSO4) and concentrated. The obtained yellow oil was purified by column chromatography (SiO2, 5-20% methanol/dichloromethane gradient elution) to afford the objective compounds as yellow oil (639 mg, 93%).

1. temperaturewith heating for 9 hours
2. temperaturecooled to 25° C.
3. concentrationconcentrated
4. customto afford a yellow solid
5. customThe resulting residue was partitioned between H2O (5 mL) and ethyl acetate (50 mL)
6. extractionthe aqueous layer was extracted with ethyl acetate (50 mL×2)
7. washwashed with brine (20 mL)
8. dry with materialdried (over MgSO4)
9. concentrationconcentrated
10. customThe obtained yellow oil was purified by column chromatography (SiO2, 5-20% methanol/dichloromethane gradient elution)