反应详情

To a suspension of 1-acetyl-4-aminopiperidine hydrochloride (715 mg) in dichloromethane (7 ml) were added diisopropylethylamine (1.83 ml) and a solution of 4-fluorobenzoyl chloride (0.83 mg) in dichloromethane (2 ml) at ambient temperature. After stirring for 6.5 hours, the reaction mixture was diluted with dichloromethane and washed with water, saturated aqueous sodium hydrogen carbonate, and brine. After drying with magnesium sulfate, the solvents were removed under reduced pressure. A residue was purified by column chromatography (silica gel 50 ml, dichloromethane:methanol=50:1 to 10:1). After rinse with diisopropyl ether, N-(1-acetylpiperidin-4-yl)-4-fluorobenzamide (738 mg) was obtained.

1. customat ambient temperature
2. washwashed with water, saturated aqueous sodium hydrogen carbonate, and brine
3. dry with materialAfter drying with magnesium sulfate
4. customthe solvents were removed under reduced pressure
5. customA residue was purified by column chromatography (silica gel 50 ml, dichloromethane:methanol=50:1 to 10:1)
6. washAfter rinse with diisopropyl ether