反应详情

To a mixture of sodium hydride (60%, 59.6 mg) in DMF (5 mL) was added ethyl 2-oxo-3-(3,4,5-trifluorophenoxy)piperidine-3-carboxylate (430 mg) at 0° C. under a nitrogen atmosphere, and the mixture was stirred for 30 min. To the reaction mixture was added 4-methoxybenzyl chloride (0.221 mL), the mixture was stirred at 0° C. for 30 min and diluted with saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The organic layer was separated, washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (352 mg).

1. stirringthe mixture was stirred at 0° C. for 30 min
2. extractionthe mixture was extracted with ethyl acetate
3. customThe organic layer was separated
4. washwashed with water and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe solvent was evaporated under reduced pressure
7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)