反应详情

A mixture of 2-amino-5-nitrobenzoic acid (475 mg), 2,5-dimethoxytetrahydrofuran (345 mg) and acetic acid (10 ml) was heated under reflux for 3 hours and then concentrated at reduced pressure. Brine was added to the resulting residue and the mixture was extracted with ethyl acetate. The organic layer was dried with anhydrous sodium sulfate and then concentrated at reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:1) to give the titled compound (yield, 73%).

1. temperaturewas heated
2. temperatureunder reflux for 3 hours
3. concentrationconcentrated at reduced pressure
4. additionBrine was added to the resulting residue
5. extractionthe mixture was extracted with ethyl acetate
6. dry with materialThe organic layer was dried with anhydrous sodium sulfate
7. concentrationconcentrated at reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:1)