反应详情

To a solution of tert-butyl (3-fluoro-4-hydroxyphenyl)carbamate (17.2 g, 75.7 mmol) in dimethyl sulfoxide (100 mL) were added 2-chloro-5-nitropyridine (10 g, 63.1 mmol) and cesium carbonate (30.8 g, 94.6 mmol), and the mixture was stirred at room temperature for 4 hr. Water was added to the reaction mixture, and the mixture was extracted twice with ethyl acetate. The combined organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and filtered. The solvent was evaporated under reduced pressure, and the residue was washed with hexane/ethyl acetate (=5/1) and collected by filtration to give the title compound (17.0 g, 77%).

1. extractionthe mixture was extracted twice with ethyl acetate
2. washThe combined organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. customThe solvent was evaporated under reduced pressure
6. washthe residue was washed with hexane/ethyl acetate (=5/1)
7. filtrationcollected by filtration