反应详情

温度

140 °C

To a solution of 3,4-dichlorophenylacetophenone (5.3 g; 20 mmoles) in glacial acetic acid (90 ml), polyphosphoric acid (64 g) was added and the resulting solution heated at 140° C. or 24 hours. After cooling, the reaction mixture was poured into ice-water, extracted with ethyl acetate (3×75 ml), the organic solution dried (Na2SO4) and the solvent removed under reduced pressure. The obtained residue was purified by column chromatography with silica gel and n-hexane-ethyl acetate 3:2 as eluent. 3-(3,4-dichlorophenyl)-2-phenyl-6-methylpyran-4-one (1.68 g) was obtained, m.p. 104° C.

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate (3×75 ml)
3. dry with materialthe organic solution dried (Na2SO4)
4. customthe solvent removed under reduced pressure
5. customThe obtained residue was purified by column chromatography with silica gel and n-hexane-ethyl acetate 3:2 as eluent