反应详情

In a 1 L round bottom flask, 4-(4-hydroxyphenyl)-4-oxo-butyric acid ethyl ester (8.65 g, 39.0 mmol), 1-bromo-3-chloro-propane (6.1 g, 61.0 mmol), and potassium carbonate (9.3 g, 67.1 mmol) in acetonitrile (300 mL) was heated to reflux 14 h. The reaction was cooled and the solvent concentrated under vacuum. The slurry was partitioned between methylene chloride and water, separated and dried over MgSO4. Purification with silica gel chromatography eluting with hexanes/ethyl acetate (3:1) produced 7.9 g (68%). MS m/z 299 (M+H).

1. temperatureto reflux 14 h
2. temperatureThe reaction was cooled
3. concentrationthe solvent concentrated under vacuum
4. customThe slurry was partitioned between methylene chloride and water
5. customseparated
6. dry with materialdried over MgSO4
7. customPurification with silica gel chromatography
8. washeluting with hexanes/ethyl acetate (3:1)
9. customproduced 7.9 g (68%)