反应详情

温度

10 °C

Under a stream of N2 and with cooling, Na metal (2.7 g) was added to MeOH (36 ml) with a considerable exotherm. After the Na is dissolved, a solution of 2-chloro-4-cyanopyridine (15 g) in dioxane:MeOH (1:1, 110 ml) was added via dropping funnel over a 10 min period. The reaction was heated to reflux for 3.5 h then cooled at ˜10° C. overnight. Solid was filtered off and the solid was washed with MeOH. The filtrate was concentrated to ˜60 ml and H2O (60 ml) was added to redissolve a precipitate. Upon further concentration, a precipitate formed which was washed with H2O. Further concentration produced additional solids. The solids were combined and dried in vacuo overnight at 35° C. to provide 4-cyano-2-methoxypyridine which was used as is.

1. customover a 10 min
2. temperatureThe reaction was heated
3. temperatureto reflux for 3.5 h
4. filtrationSolid was filtered off
5. washthe solid was washed with MeOH
6. concentrationThe filtrate was concentrated to ˜60 ml and H2O (60 ml)
7. additionwas added
8. dissolutionto redissolve a precipitate
9. concentrationUpon further concentration
10. customa precipitate formed which
11. washwas washed with H2O
12. concentrationFurther concentration
13. customproduced additional solids
14. customdried in vacuo overnight at 35° C.