反应详情

温度

80 °C

To a solution of 1-[2,4-bis(trifluoromethyl)benzyl]-2-oxopiperidine-4-carbaldehyde (1.00 g) and 4-(prop-2-yn-1-ylamino)-1,3-thiazol-2(5H)-one (0.66 g) in 2-propanol (10 mL) was added piperidinium acetate (0.41 g). The reaction mixture was stirred at 80° C. for 4 hr and concentrated. Ethyl acetate was added to the residue, and the precipitate was removed. Water was added to the filtrate, 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 (ethyl acetate/hexane) and recrystallized from ethanol/heptane to give the title compound (0.48 g).

1. concentrationconcentrated
2. additionEthyl acetate was added to the residue
3. customthe precipitate was removed
4. additionWater was added to the filtrate
5. extractionthe mixture was extracted with ethyl acetate
6. washThe extract was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was evaporated under reduced pressure
9. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
10. customrecrystallized from ethanol/heptane