反应详情

Mix together [4-(4-chloro-1-oxobutyl)phenyl]methyl-propanedioic acid, diethyl ester (380 mg, 1.1 mmol), potassium carbonate (450 mg, 3.2 mmol), α-(4-pyridyl)benzhydrol (500 mg, 1.9 mmol), water (4 mL) and toluene (10 mL). Heat the mixture to reflux. After 7 days, cool to room temperature. Add ethyl acetate and water. Wash the organic phase with brine, dry over anhydrous magnesium sulfate and concentrate. Purify by flash chromatography (200 g of silica gel, 10% methanol/chloroform as eluent) to give the title compound (627 mg, 99%).

1. temperatureHeat the mixture
2. temperatureto reflux
3. washWash the organic phase with brine
4. dry with materialdry over anhydrous magnesium sulfate
5. concentrationconcentrate
6. customPurify by flash chromatography (200 g of silica gel, 10% methanol/chloroform as eluent)