反应详情

A solution of 54 g of 1-methyl-4-phenylpiperidin-4-ol in 200 ml of absolute dimethylformamide is added dropwise to a suspension of 12.6 g of sodium hydride (80% strength in oil) in 200 ml of absolute dimethylformamide at a temperature of 45° C., while stirring and with exclusion of moisture. During this addition, evolution of hydrogen occurs. When the addition has ended, the mixture is stirred at 50° C. for a further 2 hours and allowed to cool to room temperature. A solution of 49.4 g of 4-fluoronitrobenzene in 100 ml of absolute dimethylformamide is then added dropwise thereto. Stirring is continued for a further 2 hours, and the reaction mixture is then poured onto 800 ml of ice-water. The precipitate which forms is filtered off and washed with water. Recrystallization from 250 ml of ethanol yields 52 g of the title compound of m.p. 135° to 137° C.

1. additionWhen the addition
2. stirringthe mixture is stirred at 50° C. for a further 2 hours
3. stirringStirring
4. filtrationThe precipitate which forms is filtered off
5. washwashed with water
6. customRecrystallization from 250 ml of ethanol