反应详情

A mixture of 2-iodo-3-nitrobenzoic acid (31.0 g, 106 mmol) and concentrated sulfuric acid (24.9 mL, 317 mmol) in methanol (600 mL) was heated under reflux for 12 hr. The solvent was evaporated under reduced pressure and the residue was extracted with methylene chloride. The extract was washed with saturated aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by recrystallization (chloroform/hexane) to give the title compound (31.0 g, yield 95%).

1. temperaturewas heated
2. temperatureunder reflux for 12 hr
3. customThe solvent was evaporated under reduced pressure
4. extractionthe residue was extracted with methylene chloride
5. washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution and water
6. dry with materialdried over anhydrous sodium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was purified by recrystallization (chloroform/hexane)