反应详情

A mixture of 5-(5-fluoro-2-methylphenyl)-cyclohexane-1,3-dione (1.5 g) and ammonium acetate (1.6 g) in butanol(30 ml) was combined with acetylacetone (2.0 g) and heated under reflux for 3 days. The solvent was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate, washed successively with aqueous sodium hydrogen carbonate, water and saturated brine, and dried over magnesium sulfate. The mixture was concentrated under reduced pressure, and the residue was subjected to a column chromatography on a silica gel (ethyl acetate-hexane) to obtain 7-(5-fluoro-2-methylphenyl)-2,4-dimethyl-5,6,7,8-tetrahydroquinolin-5-one (1.2 g) as an oil.

1. temperatureheated
2. temperatureunder reflux for 3 days
3. distillationThe solvent was distilled off under reduced pressure
4. dissolutionthe residue was dissolved in ethyl acetate
5. washwashed successively with aqueous sodium hydrogen carbonate, water and saturated brine
6. dry with materialdried over magnesium sulfate
7. concentrationThe mixture was concentrated under reduced pressure