反应详情

温度

110 °C

A mixture of 150 mg of tert-butyl[(1R)-1-(1-naphthyl)ethyl][(4-phenylpiperidin-3-yl)methyl]carbamate, 96.2 mg of methyl 3,4,5-trifluorobenzoate, 93.3 mg of potassium carbonate, and 1.0 mL of DMSO was stirred at 110° C. for 1 hour. After cooling to room temperature, to the reaction mixture was added water, followed by extraction with ethyl acetate. The organic layer was washed with water and saturated brine in this order, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 127 mg of methyl 4-[3-({(tert-butoxycarbonyl)[(1R)-1-(1-naphthyl)ethyl]amino}methyl)-4-phenylpiperidin-1-yl]-3,5-difluorobenzoate as a colorless foamy substance. ESI+: 615

1. temperatureAfter cooling to room temperature, to the reaction mixture
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with water and saturated brine in this order
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationAfter filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (hexane-ethyl acetate)