反应详情

To a solution of 1-amino-5-(2-chlorophenyl)cyclohexen-3-one (2.7 g) in ethanol (50 ml) and toluene (150 ml) were added acetylacetoaldehyde-dimethylacetal (4.0 g) and 85% potassium hydroxide (0.67 g), and the mixture was refluxed. With intervals of 30 minutes, 85% potassium hydroxide (0.14 g) was added 3 times to the mixture. Then, the mixture was refluxed for 1 hour. Under reduced pressure, the solvent was evaporated, and to the residue was added ethyl acetate. The mixture was washed with water and saturated brine, and dried with magnesium sulfate. Under reduced pressure, the mixture was concentrated, and the residue was subjected to silica gel column chromatography (EtOAc/hexane) to give crystals of 7-(2-chlorophenyl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-one (2.5 g).

1. temperaturethe mixture was refluxed
2. temperatureThen, the mixture was refluxed for 1 hour
3. customUnder reduced pressure, the solvent was evaporated
4. additionto the residue was added ethyl acetate
5. washThe mixture was washed with water and saturated brine
6. dry with materialdried with magnesium sulfate
7. concentrationUnder reduced pressure, the mixture was concentrated