反应详情

To 2-bromo-3-fluoro-6-methylpyridine (1.0 equiv.) in H2O (30 mL) was added potassium permanganate (1.0 equiv.). The solution was heated at 100° C. for 5 hours at which time more potassium permanganate (1.0 equiv.) was added. After heating for an additional 48 hours the material was filtered through celite (4 cm×2 inches) and rinsed with H2O (150 mL). The combined aqueous was acidified with 1N HCl to pH=4, extracted with ethyl acetate (200 mL), washed with NaCl(sat.), dried over MgSO4, filtered and concentrated to yield 6-bromo-5-fluoropicolinic acid (17%) as a white solid. LCMS (m/z): 221.9 (MH+); LC Rt=2.05 min.

1. additionwas added
2. temperatureAfter heating for an additional 48 hours the material
3. filtrationwas filtered through celite (4 cm×2 inches)
4. washrinsed with H2O (150 mL)
5. extractionextracted with ethyl acetate (200 mL)
6. washwashed with NaCl(sat.)
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated