反应详情

A mixture of 2-methoxy-3-nitrobenzoic acid methyl ester (4.82 g), lithium borohydride (298 mg), trimethyl borate (0.27 ml) and anhydrous tetrahydrofuran (200 ml) was heated under reflux for 5 h. The reaction mixture was distilled under reduced pressure and ethyl acetate and water were added to the resulting residue. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and distilled under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=1:1) to give 3.18 g of the titled compound (yield, 76%).

1. temperaturewas heated
2. temperatureunder reflux for 5 h
3. distillationThe reaction mixture was distilled under reduced pressure and ethyl acetate and water
4. additionwere added to the resulting residue
5. washThe organic layer was washed with a saturated aqueous sodium chloride solution
6. dry with materialdried with anhydrous sodium sulfate
7. distillationdistilled under reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=1:1)