反应详情

To a suspension of tert-butyl {3-fluoro-4-[(5-nitropyridin-2-yl)oxy]phenyl}carbamate (15 g, 42.9 mmol) in methanol (300 mL) was added 5 wt % palladium/carbon (3.0 g), and the mixture was stirred at room temperature for 8 hr under a hydrogen atmosphere. After nitrogen substitution, insoluble material was collected by filtration and washed with methanol. The solvent of the filtrate was evaporated under reduced pressure, water was added to the residue, and the mixture was extracted with ethyl acetate/tetrahydrofuran. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered. The solvent was evaporated under reduced pressure to give the title compound (12.3 g, 90%).

1. filtrationAfter nitrogen substitution, insoluble material was collected by filtration
2. washwashed with methanol
3. customThe solvent of the filtrate was evaporated under reduced pressure, water
4. additionwas added to the residue
5. extractionthe mixture was extracted with ethyl acetate/tetrahydrofuran
6. washThe organic layer was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. customThe solvent was evaporated under reduced pressure