反应详情

To a mixture of 2.0 g of lithium aluminum hydride and 50 ml of tetrahydrofuran, was gradually added a solution of 5.0 g of 1-[β-(p-fluorobenzoyl)propionyl]-4-(p-chlorophenyl)-4-hydroxypiperidine in 40 ml of tetrahydrofuran. The mixture was stirred at room temperature for one hour, and at 60°to 65°C for 4 hours. Then 15 ml of cold water was added dropwise to the reaction mixture while the mixture was kept below 20°C in an ice bath. The precipitate was filtered off and the tetrahydrofuran was removed from the filtrate by distillation under reduced pressure. The residue was kept cooled for 2 hours and the solid matter was collected by filtration, washed with water, and dried to obtain 1-(p-fluorophenyl)-4-[4-(p-chlorophenyl)-4-hydroxypiperidino]-1 -butanol, melting at 128° - 130°C.

1. waitat 60°to 65°C for 4 hours
2. customwas kept below 20°C in an ice bath
3. filtrationThe precipitate was filtered off
4. customthe tetrahydrofuran was removed from the filtrate by distillation under reduced pressure
5. temperatureThe residue was kept cooled for 2 hours
6. filtrationthe solid matter was collected by filtration
7. washwashed with water
8. customdried