反应详情

温度

80 °C

A mixture of 1-cyano-1-(3-hydroxyphenyl)cyclobutane (1.76 g, 10 mmol), 4-(2-methylimidazol-1-yl)benzylchloride hydrochloride (2.10 g, 10 mmol) and potassium carbonate (6.90 g, 50 mmol) in DMF (80 ml) were stirred together at 80° C. for 3 hrs. Water (200 ml) was added and the mixture extracted with ethyl acetate/benzene (2/1, 100 ml×2), washed with water (100 ml×2), brine (100 ml), dried (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography (SiO2, 150 g; dichloromethane/methanol (20/1)) to afford 2.90 g (84%) of the titled compound as a clear yellow oil.

1. extractionthe mixture extracted with ethyl acetate/benzene (2/1, 100 ml×2)
2. washwashed with water (100 ml×2), brine (100 ml)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe residue was purified by column chromatography (SiO2, 150 g; dichloromethane/methanol (20/1))