反应详情

温度

-30 °C

To a solution of the 1-(2-fluoro-phenyl)-propan-1-one (99 mmol) in concentrated sulfuric acid (80 ml) cooled down to −30° C. was added slowly fuming nitric acid (8 ml) over 20 min and the solution was stirred at −30° C. for 15 min. The mixture was slowly poured into a stirred mixture of 200 ml of water and 400 g ice. The aqueous phase was extracted with ethyl acetate, the organic layer was extracted again with water and aqueous NaHCO3 1M. The organic layer was dried over Na2SO4, evaporated and the residue was purified by chromatography on silica using a mixture of heptane and ethylacetate as eluent to afford the pure nitro intermediate J. MS (ISP): m/z=198.1 [M+H]+.

1. extractionThe aqueous phase was extracted with ethyl acetate
2. extractionthe organic layer was extracted again with water and aqueous NaHCO3 1M
3. dry with materialThe organic layer was dried over Na2SO4
4. customevaporated
5. customthe residue was purified by chromatography on silica using
6. additiona mixture of heptane and ethylacetate as eluent