反应详情

To a solution of 2-methoxy-5-nitrobenzaldehyde (450 mg) in toluene (30 ml), a solution of trimethylaluminum in hexane (3.0 ml) was added dropwise under ice cooling. After stirring at room temperature for 1 h, water was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was washed successively with water and a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=2:1) to give 385 mg of the titled compound (yield, 79%).

1. extractionwas extracted with ethyl acetate
2. washThe organic layer was washed successively with water
3. dry with materiala saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=2:1)