反应详情

To a solution of 6-bromo-7-hydroxy-2,2-dimethyl-chroman-4-one (Compound 3, 2.00 g, 7.4 mmol) in acetone (100 mL) were added potassium carbonate (500 mg) and iodomethane (5.22 g, 36.8 mmol). The mixture was then heated to reflux for 2 h. After cooling to room temperature, water was added to the mixture until all solids dissolved. The resulting solution was then extracted with diethyl ether, washed with brine, dried (MgSO4) and concentrated at reduced pressure to give a yellow residue. Purification by flash chromatography (silica gel, 95:5 hexane/ethyl acetate) gained the title compound as a white solid.

1. temperatureThe mixture was then heated
2. temperatureto reflux for 2 h
3. dissolutiondissolved
4. extractionThe resulting solution was then extracted with diethyl ether
5. washwashed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated at reduced pressure
8. customto give a yellow residue
9. customPurification by flash chromatography (silica gel, 95:5 hexane/ethyl acetate)