反应详情

A mixture of 5-(2-methylphenyl)cyclohexane-1,3-dione (1.0 g) and ammonium acetate (0.42 g) in ethanol (20 ml) was stirred at room temperature for 15 minutes. To the mixture was added 3-butyn-2-one (0.54 g), and the mixture was refluxed for 16 hours. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in ethyl acetate. The solution was washed with sodium hydrogen carbonate solution, water and saturated brine, dried with magnesium sulfate and concentrated under reduced pressure, and the residue was purified with silica gel column chromatography (EtOAc/hexane) to give colorless crystals of 2,4-dimethyl-7-(2-methylphenyl)-5,6,7,8-tetrahydroquinolin-5-one (0.50 g).

1. temperaturethe mixture was refluxed for 16 hours
2. customUnder reduced pressure, the solvent was evaporated
3. dissolutionthe residue was dissolved in ethyl acetate
4. washThe solution was washed with sodium hydrogen carbonate solution, water and saturated brine
5. dry with materialdried with magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customthe residue was purified with silica gel column chromatography (EtOAc/hexane)