反应详情

1,1,1-Trifluoro-2,4-pentanedione (25.01 g, 135.3 mmol) was dissolved in acetonitrile (230 mL), followed by the addition of methyl 3-aminocrotonate (15.57 g, 135.2 mmol). The mixture was subjected to heating under reflux for 20 hours. The reaction mixture was allowed to cool down to room temperature, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (silica gel: 400 g; developer: hexane:acetone=10:1) to obtain the title compound (22.30 g, 71%) as a yellow oil.

1. temperatureto heating
2. temperatureunder reflux for 20 hours
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by column chromatography on silica gel (silica gel: 400 g; developer: hexane:acetone=10:1)