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 of ice. The aqueous phase was extracted with ethyl acetate, the organic layer was extracted again with water and aqueous 1 M NaHCO3-solution. The organic layer was dried over Na2SO4, evaporated and the residue was chromatographed on silica using a mixture of heptane and ethylacetate as eluent to afford 16.5 g of the pure nitro intermediate XII-1. MS (ESI): 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 1 M NaHCO3-solution
3. dry with materialThe organic layer was dried over Na2SO4
4. customevaporated
5. customthe residue was chromatographed on silica using
6. additiona mixture of heptane and ethylacetate as eluent