反应详情

Under a nitrogen atmosphere, to a solution of 4.95 g of tert-butyl 2-(4-bromo-2-nitrobenzoyl)-3-oxobutanoate in 30 mL of dichloromethane was added 20 mL of trifluoroacetic acid under ice-cooling. The mixture was warmed to room temperature and stirred for 2.5 hours, and then the solvent was evaporated under reduced pressure. To the residue was added ethyl acetate, and the solution was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to obtain 2.7 g of 1-(4-bromo-2-nitrophenyl)butane-1,3-dione.

1. temperaturecooling
2. customthe solvent was evaporated under reduced pressure
3. additionTo the residue was added ethyl acetate
4. washthe solution was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)