反应详情

4-(4-Fluorobenzoyl)-1-(4-nitrobenzoyl)piperidine (4.75 g) was added slowly to a stirred mixture of iron powder (4.75 g), ammonium chloride (0.57 g), water (28.5 ml), ethanol (38 ml) and methyl cellosolve (76 ml) under reflux. The resulting mixture was stirred under reflux for 30 minutes and filtered. The filtrate was concentrated in vacuo. The residue was diluted with saturated sodium bicarbonate solution and extracted twice with methylene chloride. The extract was washed with brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was recrystallized from ethanol to give 1-(4-aminobenzoyl)-4-(4-fluorobenzoyl)piperidine (3.6 g) as pale yellow crystals.

1. temperatureunder reflux
2. temperatureunder reflux for 30 minutes
3. filtrationfiltered
4. concentrationThe filtrate was concentrated in vacuo
5. additionThe residue was diluted with saturated sodium bicarbonate solution
6. extractionextracted twice with methylene chloride
7. washThe extract was washed with brine
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated in vacuo
10. customThe resulting residue was recrystallized from ethanol