反应详情

温度

85 °C

To a mixture of iodine (19.6 g, 77.3 mmol) in fuming sulfuric acid (35 mL) was added 4-methyl-3-nitro-benzoic acid (10.0 g, 55.2 mmol). The mixture was stirred at 85° C. over night, then cooled to room temperature and poured over ice. The mixture was partitioned between ethyl acetate and aqueous sodium bisulfite, and the organic layer was separated, dried over MgSO4, filterd and concentrated under reduced pressure to give 16.06 g (95%) of 3-iodo-4-methyl-5-nitro-benzoic acid.

1. temperaturecooled to room temperature
2. additionpoured over ice
3. customThe mixture was partitioned between ethyl acetate and aqueous sodium bisulfite
4. customthe organic layer was separated
5. dry with materialdried over MgSO4, filterd
6. concentrationconcentrated under reduced pressure