反应详情

O-(4-cyano-2-ethoxybenzyl)hydroxyamine hydrochloride (19-1, 2.7 g, 0.012 mol), methanol (20 ml) and water (20 ml) were charged, and a 36% formaldehyde aqueous solution was added to this, and the mixture was stirred at room temperature for 2.0 hours. Water was added to the mixture and the mixture was extracted with ethyl acetate. The resulted ethyl acetate layer was dried over anhydrous magnesium sulfate, then, the solvent was distilled off under reduce pressure. This was purified by silica gel column chromatography using hexane/ethyl acetate system, to obtain O-(4-cyano-2-ethoxybenzyl)hydroxyamine-formaldehyde derivative (3-1a, 2.2 g, yield 96%).

1. extractionthe mixture was extracted with ethyl acetate
2. dry with materialThe resulted ethyl acetate layer was dried over anhydrous magnesium sulfate
3. distillationthe solvent was distilled off
4. customThis was purified by silica gel column chromatography