反应详情

温度

120 °C

A mixture of 185 mg of tert-butyl {[1-(4-cyano-2,6-difluorophenyl)-4-phenylpiperidin-3-yl]methyl}[(1R)-1-(1-naphthyl)ethyl]carbamate, 414 mg of sodium azide, 876 mg of triethylamine hydrochloride, and 4.0 mL of DMF was stirred at 120° C. overnight. The reaction mixture was cooled to room temperature, and water added thereto, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution in this order, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure to obtain tert-butyl ({1-[2,6-difluoro-4-(1H-tetrazol-5-yl)phenyl]-4-phenylpiperidin-3-yl}methyl)[(1R)-1-(1-naphthyl)ethyl]carbamate as a crude product (beige foamy substance, 208 mg). ESI+: 625

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materiala saturated aqueous sodium chloride solution in this order, and dried over anhydrous sodium sulfate
5. filtrationAfter filtration
6. concentrationthe filtrate was concentrated under reduced pressure