反应详情

To a solution of 1-phenylbutane-1,3-dione (5.0 g, 30.8 mmol) in ethanol (50 mL), was added hydrazine hydrate (1.54 g, 30.8 mmol) at ambient temperature. The reaction was refluxed for 5 h. After cooling, the reaction was concentrated under reduced pressure and extracted with ethyl acetate. The extract was dried over MgSO4 and concentrated under reduced pressure. The residue was added 10% ethyl acetate in hexane. The precipitate was filtered and washed with hexane. The white solid was dried in air to give the title compound (3.9 g). LCMS m/z=159.3 [M+H]+; 1H NMR (400 MHz, DMSO-d6) δ ppm 2.25 (s, 3H), 6.65 (s, 1H), 7.34 (m, 1H), 7.42 (m, 2H), 7.82 (m, 2H).

1. temperatureThe reaction was refluxed for 5 h
2. temperatureAfter cooling
3. concentrationthe reaction was concentrated under reduced pressure
4. extractionextracted with ethyl acetate
5. dry with materialThe extract was dried over MgSO4
6. concentrationconcentrated under reduced pressure
7. additionThe residue was added 10% ethyl acetate in hexane
8. filtrationThe precipitate was filtered
9. washwashed with hexane
10. customThe white solid was dried in air