反应详情

Toluene (25 ml), p-toluenesulfonic acid monohydrate (10.9 mg, 57.2 μmol) were added to N-(3-bromo-6-cyano-2-hydroxy-4-iodo-5-methylphenyl)-2,2-dimethylpropionamide (I-7) (250 mg, 572 μmol), followed by refluxing with a Dean-Stark condenser for 3 hours. After cooling, saturated sodium bicarbonate water (30 ml) was added to the reaction liquid, the product was extracted with ethyl acetate (50 ml×2). The organic layer was washed with saturated brine (50 ml), dried over anhydrous magnesium sulfate, concentrated under reduced pressure, the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1) to obtain the entitled compound (225 mg, 94%) as a pale yellow solid.

1. temperatureby refluxing with a Dean-Stark condenser for 3 hours
2. temperatureAfter cooling
3. extractionthe product was extracted with ethyl acetate (50 ml×2)
4. washThe organic layer was washed with saturated brine (50 ml)
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1)