反应详情

温度

50 °C

A solution of nipecotamide (6.40 g, 50 mmol) in CH3CN (150 mL) and ethanol (20 mL) was treated with Et3N (7.0 mL, 50 mmol) and 4-chlorobenzyl chloride (8.05 g, 50 mmol). The reaction mixture was stirred at 50° C. for 16 h. After cooling to room temperature, saturated aqueous NaHCO3 (50 mL) and water (150 mL) was added to the reaction mixture. The mixture was extracted with ethyl acetate (150 mL×3) and the combined organic layers were washed with brine, dried (Na2SO4) and concentrated to give a pale red solid. The crude solid was washed with ether (100 mL) to afford 3-carbamoyl-1-(4-chlorobenzyl)piperidine (6.98 g, 54%).

1. temperatureAfter cooling to room temperature
2. extractionThe mixture was extracted with ethyl acetate (150 mL×3)
3. washthe combined organic layers were washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customto give a pale red solid
7. washThe crude solid was washed with ether (100 mL)