反应详情

To a mixture consisting of 1 g of 2-amino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid, 20 ml of benzene, and 0.7 ml of pyridine in a flask cooled with ice water was added dropwise with stirring a solution of 600 mg of acetyl chloride in 5 ml of benzene. The mixture was further stirred for 5 hours at room temperature, and then heated to reflux for one hour. After cooling, the mixture was shaken with dilute hydrochloric acid and the layers were separated. The acidic aqueous layer was extracted with ethyl acetate, and the combined organic extracts were washed with water, and dried over sodium sulfate. The solvent was removed by distillation. The resulting residue was recrystallized from ethanol/water to yield 1.02 g of 2-acetylamino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid melting at 170°-171° C.

1. additionwas added dropwise
2. temperatureheated
3. temperatureto reflux for one hour
4. temperatureAfter cooling
5. customthe layers were separated
6. extractionThe acidic aqueous layer was extracted with ethyl acetate
7. washthe combined organic extracts were washed with water
8. dry with materialdried over sodium sulfate
9. customThe solvent was removed by distillation
10. customThe resulting residue was recrystallized from ethanol/water