反应详情

5-bromo-2-hydrazinylphenol 4-methylbenzenesulfonate (0.9 g) and acetylacetone (0.8 g) were added to ethanol (25 mL) refluxed for 1 h. Then the reaction mixture was cooled to room temperature and the solvent was evaporated under reduced pressure. The residue was dissolved in ethyl acetate (50 mL) and washed with saturated sodium bicarbonate solution (20 mL×2). The organic layer was dried over anhydrous Na2SO4, and concentrated under reduced pressure. The resulting residue was chromatographed over silica gel column eluted with hexane/ethyl acetate (4:1) to yield the title compound (650 mg).

1. temperaturerefluxed for 1 h
2. customthe solvent was evaporated under reduced pressure
3. dissolutionThe residue was dissolved in ethyl acetate (50 mL)
4. washwashed with saturated sodium bicarbonate solution (20 mL×2)
5. dry with materialThe organic layer was dried over anhydrous Na2SO4
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was chromatographed over silica gel column
8. washeluted with hexane/ethyl acetate (4:1)