反应详情

2,3-Dimethyl-4-nitropyridine-1-oxide (5 g) was dissolved in methanol (30 ml). To the solution were added tetrabutylammonium bromide (0.5 g) and potassium hydrogen carbonate (5.6 g), and the mixture was heated (temperature 80°-85° C.) under reflux with stirring for 10 hours. The solid matter was removed from the reaction mixture by filtration, and the filtrate was concentrated and applied to a silica gel (100 g) column. Elution with methanol-dichloromethane (1:9) and recrystallization from ethyl acetate-hexane gave 4.3 g of white 2,3-dimethyl-4-methoxypyridine-1-oxide. Melting point 85°-86° C.

1. temperaturethe mixture was heated (temperature 80°-85° C.)
2. temperatureunder reflux
3. customThe solid matter was removed from the reaction mixture by filtration
4. concentrationthe filtrate was concentrated
5. washElution
6. customwith methanol-dichloromethane (1:9) and recrystallization from ethyl acetate-hexane