反应详情

To a solution of 7-methoxy-2,2-dimethyl-chroman-4-one (Compound 1, 5.81 g, 28.2 mmol) in anhydrous N,N-dimethylformamide (15 mL) under argon at 25° C. was added N-bromosuccinimide (5.02 g, 33.8 mmol). The mixture was stirred at ambient temperature for 12 h. The product was extracted with diethyl ether. The organic layers were washed with water, brine, and dried over Na2SO4. The filtered solvent was concentrated in vacuo and purified by column chromatography (silica gel, 5% ethyl acetate in hexane) to give the title compound as a white solid.

1. extractionThe product was extracted with diethyl ether
2. washThe organic layers were washed with water, brine
3. dry with materialdried over Na2SO4
4. concentrationThe filtered solvent was concentrated in vacuo
5. custompurified by column chromatography (silica gel, 5% ethyl acetate in hexane)