반응 #78051

반응 방정식

1-benzyl-4-aminopiperidine

4-fluorobenzoyl chloride

→

N-(1-benzylpiperidin-4-yl)-4-fluorobenzamide

수율 70.6%

용매

dichloromethane

dichloromethane

dichloromethane

diisopropylethylamine

반응 조건

후처리

1. 1
   온도under cooling on an ice-water bath
2. 2
   세척washed with water, saturated aqueous sodium hydrogen carbonate, water, and brine
3. 3
   건조After drying with magnesium sulfate
4. 4
   기타the solvents were removed under reduced pressure
5. 5
   기타A residue was purified by column chromatography (silica gel 100 ml, dichloromethane:methanol=15:1)
6. 6
   세척After rinse with diisopropyl ether-n-hexane (1:1)

실험 절차

To a solution of 1-benzyl-4-aminopiperidine (1.13 g) in dichloromethane (10 ml) were added a solution of 4-fluorobenzoyl chloride (0.99 g) in dichloromethane (1 ml) and diisopropylethylamine (1.09 ml) under cooling on an ice-water bath. The mixture was warmed to ambient temperature slowly under stirring. The mixture was diluted with dichloromethane and washed with water, saturated aqueous sodium hydrogen carbonate, water, and brine. After drying with magnesium sulfate, the solvents were removed under reduced pressure. A residue was purified by column chromatography (silica gel 100 ml, dichloromethane:methanol=15:1). After rinse with diisopropyl ether-n-hexane (1:1), N-(1-benzylpiperidin-4-yl)-4-fluorobenzamide (1.31 g) was obtained.

출처