反应详情

To a solution of (3,5-dichloro-4-hydroxy-phenyl)-carbamic acid tert-butyl ester (1.0 g) and potassium carbonate (0.55 g) in toluene (20 mL) is added ethylene carbonate (1.6 g) and the mixture is heated to reflux for 3 hours. To the cooled reaction mixture is added 2.5 M aqueous sodium hydroxide (50 mL), and the separated organic layer is then washed successively with water, then saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate. The solvent is then removed by evaporation under reduced pressure and the resulting residue is chromatographed over silica gel (30% ethyl acetate in hexanes is used as the eluant) to provide the desired product as a white foam.

1. temperaturethe mixture is heated
2. temperatureto reflux for 3 hours
3. customTo the cooled reaction mixture
4. washthe separated organic layer is then washed successively with water
5. dry with materialsaturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate
6. customThe solvent is then removed by evaporation under reduced pressure
7. customthe resulting residue is chromatographed over silica gel (30% ethyl acetate in hexanes