反应详情

温度

60 °C

To a solution of 1-{1-[2,4-bis(trifluoromethyl)phenyl]ethyl}piperidine-4-carbaldehyde (1.15 g) and 4-(prop-2-yn-1-ylamino)-1,3-thiazol-2(5H)-one (1.00 g) in 2-propanol (16.3 mL) was added piperidinium acetate (0.473 g). The reaction mixture was stirred at 60° C. overnight, allowed to cool to room temperature, and diluted with ethyl acetate. The mixture was 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 (NH, ethyl acetate/hexane), further purified by silica gel column chromatography (ethyl acetate/hexane), and recrystallized from ethyl acetate/hexane to give the title compound (1.13 g).

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