反应详情

4-Bromo-benzaldehyde (available from Aldrich, 10.0 g, 54.3 mmol) was added to a solution of 3-methyl-butan-2-one (available from Aldrich, 4.7 g, 54.7 mmol) in 10 mL of 10% NaOH(aq) and 20 mL of ethanol. After stirring at room temperature for 3 h, the reaction mixture was diluted with water (50 mL) and extracted with diethyl ether (3×20 mL). The organic layer was then washed with brine (1×5 mL), dried (MgSO4) and concentrated at reduced pressure. Purification by flash chromatography (95:5 hexane/ethyl acetate) yielded the title compound (7.98 g, 58% yield) as a light yellow oil:

1. extractionextracted with diethyl ether (3×20 mL)
2. washThe organic layer was then washed with brine (1×5 mL)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated at reduced pressure
5. customPurification by flash chromatography (95:5 hexane/ethyl acetate)