反应详情

A mixture of 5-phenylcyclohexane-1,3-dione (1.0 g) and ammonium acetate (0.45 g) in ethanol (30 ml) was stirred at room temperature for 1 hour, refluxed for 6 hours and cooled. To the reaction solution was added ethyl propiolate (0.55 g), and the mixture was stirred at room temperature for 1 hour and refluxed 14.5 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 recrystallized from ethanol to give colorless crystals of 7-phenyl-1,2,5,6,7,8-hexahydroquinoline-2,5-dione (0.19 g).

1. temperaturerefluxed for 6 hours
2. temperaturecooled
3. stirringthe mixture was stirred at room temperature for 1 hour
4. temperaturerefluxed 14.5 hours
5. customUnder reduced pressure, the solvent was evaporated
6. dissolutionthe residue was dissolved in ethyl acetate
7. washThe solution was washed with sodium hydrogen carbonate solution, water and saturated brine
8. dry with materialdried with magnesium sulfate
9. concentrationconcentrated under reduced pressure
10. customthe residue was recrystallized from ethanol