反应详情

温度

80 °C

69 mg of O-methylhydroxylamine hydrochloride were added to a solution of 0.12 g (0.41 mmol) of 4'-nitro-2-t-butyldimethylsilyloxyacetophenone (obtained above) in a mixture of methanol (1.2 ml), 1,4-dioxane (2.0 ml) and water (2.0 ml). The resulting mixture was stirred for 1.5 hours at 80° C., then poured into water and extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The residue was purified by silica gel column chromatography, eluted with a stepwise gradient of ethyl acetate (10-40%) in hexane, to give 58 mg (67% yield) of the title compound.

1. extractionextracted with ethyl acetate
2. washThe extract was washed with a saturated aqueous solution of sodium chloride
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe residue was purified by silica gel column chromatography
5. washeluted with a stepwise gradient of ethyl acetate (10-40%) in hexane