反应详情

温度

100 °C

To 6-bromo-3-fluoro-2-methylpyridine (2.0 g, 10.58 mmoles) in H2O (200 mL) was added potassium permanganate (1.67 g, 10.58 mmoles). The solution was heated at 100° C. for 16 hours at which time upon cooling 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 pH4, extracted with ethyl acetate (2×200 mL), washed with NaCl(sat.), dried over MgSO4, filtered and concentrated to yield 6-bromo-3-fluoropicolinic acid (18%) as a white solid. LCMS (m/z): 221.9 (MH+); LC Rt=1.71 min.

1. temperatureupon cooling the material
2. filtrationwas filtered through celite (4 cm×2 inches)
3. washrinsed with H2O (150 mL)
4. extractionextracted with ethyl acetate (2×200 mL)
5. washwashed with NaCl(sat.)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated