反应详情

温度

80 °C

To 1-(4-fluoro-2-hydroxyphenyl)ethanone (5.75 g, 37.3 mmol) and propan-2-one (12 mL, 37.3 mmol) in benzene (50 mL) was added pyrrolidine (3.11 mL, 37.3 mmol) and the reaction heated at 80° C. for 3 hours. The reaction was diluted with ethyl acetate (50 mL), washed with 1N HCl (50 mL), brine (50 mL), dried over magnesium sulfate and concentrated. The residue was purified by silica gel chromatography, eluting with a gradient of 5% ethyl acetate/hexanes to 50% ethyl acetate, to provide the title compound (5.12 g, 70.7% yield).

1. washwashed with 1N HCl (50 mL), brine (50 mL)
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated
4. customThe residue was purified by silica gel chromatography
5. washeluting with a gradient of 5% ethyl acetate/hexanes to 50% ethyl acetate