反应详情

温度

60 °C

To a solution of 1-[2,4-bis(trifluoromethyl)benzyl]azepane-4-carbaldehyde (156.5 mg) in 2-propanol (2.22 mL) were added 4-(prop-2-yn-1-ylamino)-1,3-thiazol-2(5H)-one (137 mg) and piperidinium acetate (64.3 mg). The reaction mixture was stirred at 60° C. overnight, allowed to cool to room temperature, poured into saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with 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 (NH, ethyl acetate/hexane) and recrystallized from ethyl acetate/hexane to give the title compound (63.0 mg).

1. temperatureto cool to room temperature
2. extractionthe mixture was extracted with ethyl acetate
3. washThe extract was washed with saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was evaporated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)
7. customrecrystallized from ethyl acetate/hexane