反应详情

A solution of 5-iodo-2,4-dimethylbenzoic acid (compound 2.1, 10 g, 32.60 mmol, 1.00 equiv, 90%) and sulfuric acid (10 mL) in methanol (100 mL) was stirred overnight at 80° C. After cooling to room temperature, the mixture was concentrated under reduced pressure and the residue was diluted with 200 mL of ethyl acetate. The resulting mixture was washed with 3×50 mL of water, 2×50 mL of sodium bicarbonate (aq. sat.), followed by 2×50 mL of brine. The organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure to yield 9.2 g (88%) of the title compound as a yellow oil.

1. concentrationthe mixture was concentrated under reduced pressure
2. additionthe residue was diluted with 200 mL of ethyl acetate
3. washThe resulting mixture was washed with 3×50 mL of water, 2×50 mL of sodium bicarbonate (aq. sat.)
4. dry with materialThe organic phase was dried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure