反应详情

温度

75 °C

1-(4-fluoro-2-hydroxyphenyl)ethanone (12.0 g, 77.9 mmol), iodomethane (6.38 ml, 101 mmol), potassiumcarbonate (14.0 g, 101 mmol) were heated at 75° C. in ACN (200 ml) for 8 h. The reaction mixture was brought to ambient temperature, filtered and then evaporated under reduced pressure to dryness. New ACN (150 ml), iodomethane (2 ml, 32 mmol) and potassiumcarbonate (4 g, 29 mmol) was added. The reaction mixture was heated at 75° C. for 3 h. The reaction mixture was concentrated, EtOAc (100 ml) was added and the mixture was filtered and evaporated to give the title product (13.5 g, 100%). MS m/z (rel. intensity, 70 eV) 168 (M+, 11), 153 (bp), 110 (23), 95 (21), 82 (12).

1. customwas brought to ambient temperature
2. filtrationfiltered
3. customevaporated under reduced pressure to dryness
4. concentrationThe reaction mixture was concentrated
5. additionEtOAc (100 ml) was added
6. filtrationthe mixture was filtered
7. customevaporated