反应详情

To acetic acid solution (15 ml) of 7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one (2.82 g, 8.99 mmol) was added aqueous 48% HBr solution (13 ml) and the mixture was heated under refluxing for 24 hours. The reaction solution was extracted with ethyl acetate, and the organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated saline, dried over anhydrous magnesium sulfate and then distilled under reduced pressure to remove the solvent. The crude product thus obtained was purified with silica gel column chromatography (ethyl acetate:hexane=2:1) to obtain 2.46 g (yield: 96%) of the title compound.

1. temperaturethe mixture was heated
2. temperatureunder refluxing for 24 hours
3. extractionThe reaction solution was extracted with ethyl acetate
4. washthe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated saline
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationdistilled under reduced pressure
7. customto remove the solvent
8. customThe crude product thus obtained
9. customwas purified with silica gel column chromatography (ethyl acetate:hexane=2:1)