反应详情

温度

140 °C

To a solution of 2-(4-fluorophenyl)-1-(4-methanesulfonylphenyl)ethanone (1 g; 3.4 moles) in glacial acetic acid (15 ml), polyphosphoric acid (10 g) was added and then heated at 140° C. for 16 hours. After cooling, the reaction was poured into ice-water, extracted with ethyl acetate (2×50 ml), the organic solution dried (Na2SO4) and the solvent removed under reduced pressure. The residual oil was purified by column chromatography with silica gel and ethyl acetate as eluent. 3-(4-fluorophenyl)-2-(4-methanesulfonylphenyl)-6-methylpyran-4-one was obtained (0.5 g) m.p. 237° C. (Compound 2 in Table 4).

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate (2×50 ml)
3. dry with materialthe organic solution dried (Na2SO4)
4. customthe solvent removed under reduced pressure
5. customThe residual oil was purified by column chromatography with silica gel and ethyl acetate as eluent