反应详情

A solution of [3-chloro-4-(3-dimethylamino-acryloyl)-phenyl]-carbamic acid tert-butyl ester (270 mg) in dioxane (3 ml) is treated with hydroxylamine hydrochloride (122 mg) and the mixture is stirred at room temperature for 10 days. The mixture is diluted with ethyl acetate, washed successively with water, 5% aqueous sodium bicarbonate, saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. The solvent is removed by evaporation under reduced pressure and the resulting residue is chromatographed over silica gel (33% ethyl acetate in hexanes is used as the eluant) to provide the desired product as a colorless solid.

1. washwashed successively with water, 5% aqueous sodium bicarbonate, saturated aqueous sodium chloride
2. dry with materialdried over anhydrous magnesium sulfate
3. customThe solvent is removed by evaporation under reduced pressure
4. customthe resulting residue is chromatographed over silica gel (33% ethyl acetate in hexanes