反应详情

4-Benzyloxypyridine 1-oxide (24.8 g, 123 mmols) was refluxed in acetic anhydride (150 mL) for 1.5 hours. Cooling the system to room temperature, the system was concentrated under reduced pressure and the resulting residue was dissolved in a mixed solvent of ethyl acetate (150 mL) and methanol (10 mL), followed by stirring at 60° C. for 2 hours. The solid formed upon cooling the system to room temperature was recovered by filtration to provide crude title compound (8.84 g). Concentrating the filtrate, additional crude title compound (4.17 g) was obtained. The combined crude product was recrystallized from a mixed solvent of methanol and ethyl acetate to provide the title compound (12.1 g, 49%).

1. concentrationthe system was concentrated under reduced pressure
2. dissolutionthe resulting residue was dissolved in a mixed solvent of ethyl acetate (150 mL) and methanol (10 mL)
3. customThe solid formed
4. temperatureupon cooling the system to room temperature
5. filtrationwas recovered by filtration
6. customto provide crude title compound (8.84 g)
7. concentrationConcentrating the filtrate
8. customadditional crude title compound (4.17 g) was obtained
9. customwas recrystallized from a mixed solvent of methanol and ethyl acetate