反应详情

To the dichloromethane (70 ml) solution of 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 3 g, 14.7 mmol), acetic anhydride (1.7 ml, 1.2 eq.) and aluminum chloride-nitrobenzene solution (1 M, 44 ml, 3 eq.) was added at 0° C., and stirred for 3 hr. Thereafter, the reaction solution was added with saturated aqueous solution of sodium hydrogen carbonate and extracted twice with dichloromethane. The organic layer was washed with brine and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound as a crude product.

1. extractionextracted twice with dichloromethane
2. washThe organic layer was washed with brine
3. dry with materialdried over magnesium sulfate
4. customThe drying agent was removed by filtration
5. customthe residues obtained
6. concentrationafter concentration under reduced pressure
7. customwere purified by silica gel column chromatography (ethyl acetate/hexane)