反应详情

Trifluoroacetic acid(5 mL) is added to solid (3,5-dichloro-4-ethoxy-phenyl)-carbamic acid tert-butyl ester (0.97 g) and the mixture is stirred for approximately 45 minutes at room temperature. Water is then added, and the mixture is cooled in an ice bath and basified with solid potassium carbonate. The solution is extracted three times with ethyl acetate and the combined organic phases are washed with saturated aqueous sodium chloride then dried over anhydrous sodium sulfate. Concentration under reduced pressure and recrystallization from hexanes provides the desired product as a pale yellow crystalline solid.

1. temperaturethe mixture is cooled in an ice bath
2. extractionThe solution is extracted three times with ethyl acetate
3. washthe combined organic phases are washed with saturated aqueous sodium chloride
4. dry with materialthen dried over anhydrous sodium sulfate
5. concentrationConcentration
6. customunder reduced pressure and recrystallization from hexanes