反应详情

To a mixture of 2-methoxy-6-nitroaniline (5.9 g) in valeric anhydride (14 g) was added a catalytic amount of conc. sulfuric acid, which was stirred for 1.5 hour at 130°-140° C. To the reaction mixture was added water, which was made basic with 6N NaOH. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with water and dried. The solvent was distilled off. The residue was purified by column chromatography on silica gel. Crude crystals thus obtained were recrystallized from ethyl acetate-hexane to give colorless crystals (3.2 g, 36%), m.p. 113°-114° C.

1. extractionThe reaction mixture was extracted with ethyl acetate
2. washThe organic layer was washed with water
3. customdried
4. distillationThe solvent was distilled off
5. customThe residue was purified by column chromatography on silica gel
6. customCrude crystals thus obtained
7. customwere recrystallized from ethyl acetate-hexane