反应详情

p-Toluenesulfonic acid monohydrate (0.070 g) was added to a suspension of the compound prepared in Example 95 (0.56 g) in toluene (20 mL). The reaction mixture was heated at reflux under Dean-Stark conditions overnight. The reaction mixture was then cooled to room temperature and partitioned between dichloromethane and a saturated aqueous sodium bicarbonate solution. The combined organics were dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:hexane=3:2) to obtain the title compound (0.35 g) having the following physical data.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux under Dean-Stark conditions overnight
3. custompartitioned between dichloromethane
4. dry with materialThe combined organics were dried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customThe residue was purified by column chromatography on silica gel (ethyl acetate:hexane=3:2)