反应详情

Nine milliliters of acetyl chloride were added to a mixture of 18.4 g of ethyl 3-amino-4-nitrobenzoate and 200 ml of N,N-dimethylaniline while being cooled with ice. The mixture was stirred at room temperature for 2 hours and then at 50° C. for 2 hours. The reaction solution was poured into cold 1-N hydrochloric acid, and the mixture was extracted twice with ethyl acetate. The organic layer was washed with 1-N hydrochloric acid and then with water, and was dried. The solvent was then distilled off under reduced pressure. The residue was purified through silica-gel column chromatography (eluent: a mixture of ethyl acetate and hexane at a ratio of from 1:10 to 1:4) to give 19.6 g of ethyl 3-acetylamino-4-nitrobenzoate.

1. temperaturewhile being cooled with ice
2. waitat 50° C. for 2 hours
3. extractionthe mixture was extracted twice with ethyl acetate
4. washThe organic layer was washed with 1-N hydrochloric acid
5. dry with materialwith water, and was dried
6. distillationThe solvent was then distilled off under reduced pressure
7. customThe residue was purified through silica-gel column chromatography (eluent
8. additiona mixture of ethyl acetate and hexane at a ratio of from 1:10 to 1:4)