反应详情

Concentrated sulfuric acid (12 ml) was added to a solution of 2-methyl-5-nitrobenzoic acid (10.87 g) in ethanol (60 ml). The mixture was heated under reflux overnight. The reaction solution was concentrated under the reduced pressure. Water was then added to the residue. The mixture was extracted with diethyl ether. The extract was washed with water and saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under the reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1) to give ethyl 2-methyl-5-nitrobenzoate (11.86 g).

1. temperatureThe mixture was heated
2. temperatureunder reflux overnight
3. concentrationThe reaction solution was concentrated under the reduced pressure
4. additionWater was then added to the residue
5. extractionThe mixture was extracted with diethyl ether
6. washThe extract was washed with water and saturated saline
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was then removed by distillation under the reduced pressure
9. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1)