反应详情

0.3 ml of acetic anhydride and 100 mg of 10% palladium-carbon catalyst were added to an ethanol (20 ml) solution of 300 mg of t-butyl (4-(4-fluoro-phenoxy)-3-pyridin-2-yl-phenyl)-carbamate, and the reaction liquid was stirred overnight in a hydrogen atmosphere. The catalyst was removed through filtration through Celite, and the filtrate was distilled under reduced pressure to obtain a crude product. The resulting crude product was dissolved in 5 ml of 4 N hydrochloric acid/1,4-dioxane solution, and the reaction liquid was stirred at room temperature for 1 hour. Aqueous saturated sodium bicarbonate was added to the reaction liquid, and extracted with ethyl acetate. The organic layer was washed with saturated saline, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate) to obtain the entitled compound as a pale yellow solid.

1. customthe reaction liquid
2. customThe catalyst was removed through filtration through Celite
3. distillationthe filtrate was distilled under reduced pressure
4. customto obtain a crude product
5. customthe reaction liquid
6. extractionextracted with ethyl acetate
7. washThe organic layer was washed with saturated saline
8. dry with materialdried with anhydrous sodium sulfate
9. customThe solvent was evaporated away under reduced pressure
10. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate)