反应详情

To a solution of 3-amino-5-hydroxy-4-iodo-benzoic acid (0.20 g, 0.72 mmol) in methanol (5 mL) was added conc. sulfuric acid (0.20 mL, 0.035 g, 0.36 mmol) and the reaction mixture heated to reflux. After 2 h, the reaction mixture was poured on ice, the pH adjusted to 9 by addition of a sat. solution of sodium hydrogencarbonate and extracted with ethyl acetate (2×50 mL). The combined organic phases were dried over MgSO4, concentrated by evaporation under reduced pressure and the crude material purified with column chromatography on silica eluting with hexane/ethyl acetate (1:1) providing 0.07 g (33%) of the title compound.

1. temperaturethe reaction mixture heated to reflux
2. additionthe reaction mixture was poured on ice
3. extractionextracted with ethyl acetate (2×50 mL)
4. dry with materialThe combined organic phases were dried over MgSO4
5. concentrationconcentrated by evaporation under reduced pressure
6. customthe crude material purified with column chromatography on silica eluting with hexane/ethyl acetate (1:1)