反应详情

A mixture of 3-amino-4-chlorophenol (5.0 g), 3-(4-chlorophenylsulfanyl)pentane-2,4-dione (8.4 g), p-toluenesulfonic acid monohydrate (3.20 g) and toluene (150 mL) was heated at reflux for 2 days. The mixture was cooled to room temperature and the solvent removed under reduced pressure. The residue was dissolved in ethyl acetate, washed with water and saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel, eluting with a mixture of dichloromethane and cyclohexane (1:9 by volume) gave title compound as a pale yellow solid, 0.99 g.

1. temperaturewas heated
2. temperatureat reflux for 2 days
3. customthe solvent removed under reduced pressure
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with water and saturated aqueous sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. customThe solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel
8. washeluting with a mixture of dichloromethane and cyclohexane (1:9 by volume)