反应详情

To a suspension of 4-amino-3-methylbenzoic acid (5.00 g, 33.1 mmol) in ethanol (50 ml), concentrated sulfuric acid (5.00 ml) was slowly added. The mixture was heated under reflux for 3 hours. The solvent was distilled off under a reduced pressure. After the volume of the mixture was approximately halved, the mixture was neutralized with a saturated sodium bicarbonate solution. The mixture was subjected to extraction with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and then concentrated to give the title compound (5.87 g, 99%) as a light-brown solid.

1. additionwas slowly added
2. temperatureThe mixture was heated
3. temperatureunder reflux for 3 hours
4. distillationThe solvent was distilled off under a reduced pressure
5. extractionThe mixture was subjected to extraction with ethyl acetate
6. dry with materialthe extract was dried over anhydrous magnesium sulfate
7. concentrationconcentrated