反应详情

To a mixture of nitric acid (d=1.42:20 ml) and sulfuric acid (d=1.84:20 ml) was added 2,3-dimethyl benzoic acid (6.0 g) at 0° C. After stirring for 3 hours, the mixture was poured into ice water (300 ml). The organic layer was extracted with ethyl acetate (100 ml) and washed with water (100 ml×3). The solution was dried over magnesium sulfate and the solvent was removed in vacuo. The residue was purified by a column of silica gel to give a yellow solid of 2,3-dimethyl-5-nitrobenzoic acid (1.80 g).

1. extractionThe organic layer was extracted with ethyl acetate (100 ml)
2. washwashed with water (100 ml×3)
3. dry with materialThe solution was dried over magnesium sulfate
4. customthe solvent was removed in vacuo
5. customThe residue was purified by a column of silica gel