反应详情

温度

50 °C

Triethylamine (7.0 mL, 50 mmol) and 4-chlorobenzyl chloride (8.05 g, 50 mmol) were added to a solution of nipecotamide (6.40 g, 50 mmol) in acetonitrile (150 mL) and ethanol (20 mL). The resulting reaction mixture was stirred at 50° C. for 16 hours and cooled to room temperature. A saturated aqueous solution of NaHCO3 (50 mL) and water (150 mL) were then added, and the resulting mixture was extracted with ethyl acetate (150 mL×3). The extracts were washed with brine, dried over Na2SO4 and concentrated to afford a light-red solid. The obtained crude solid was washed with ether (100 mL) to provide 3-carbamoyl-1-(4-chlorobenzyl)piperidine (6.98 g, 54%).

1. customThe resulting reaction mixture
2. temperaturecooled to room temperature
3. extractionthe resulting mixture was extracted with ethyl acetate (150 mL×3)
4. washThe extracts were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customto afford a light-red solid
8. customThe obtained crude solid
9. washwas washed with ether (100 mL)