反应详情

To a solution of 9.1 g of 60% oily sodium hydride in 200 ml of tetrahydrofuran, 38.0 ml of ethyl diethylphosphonoacetate was added dropwise under cooling with ice, stirred for 20 minutes, and thereafter a solution of 31.4 g of 1-t-butoxycarbonyl-4-piperidone in 500 ml of tetrahydrofuran was added dropwise, followed by 40 minutes' stirring at the same temperature. The reaction liquid was diluted with ethyl acetate, washed successively with aqueous ammonium chloride solution, water and saturated brine, and dried over anhydrous sodium sulfate. Distilling the solvent off under reduced pressure, the residue was recrystallized from methanol to provide 33.5 g of the title compound.

1. temperatureunder cooling with ice
2. waitfollowed by 40 minutes
3. stirring' stirring at the same temperature
4. customThe reaction liquid
5. washwashed successively with aqueous ammonium chloride solution, water and saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. distillationDistilling the solvent off under reduced pressure
8. customthe residue was recrystallized from methanol