反应详情

To 5-bromo-3-(2-methylpyridin-3-yloxy)picolinonitrile (15 g, 52 mmol) was added concentrated H2SO4 (30 mL) and the slurry was stirred overnight, at which point the material was fully dissolved. The reaction was poured into 0° C. water in small portions. While maintaining the temp below 20° C., the aqueous layer was basified to about a pH of 5 by the addition of NaOH pellet, at which point a solid formed. The solid was filtered, and the remaining aqueous layer was extracted with EtOAc. The organics layers, combined with the solid, were washed with brine, dried over MgSO4 and concentrated in vacuo to yield 5-bromo-3-(2-methylpyridin-3-yloxy)picolinamide (11 g, 69%).

1. dissolutionwas fully dissolved
2. temperatureWhile maintaining the temp below 20° C.
3. customformed
4. filtrationThe solid was filtered
5. extractionthe remaining aqueous layer was extracted with EtOAc
6. washwere washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo