반응 #157124

반응 방정식

6-bromo-3-fluoro-2-methylpyridine

potassium permanganate

H2O

→

6-bromo-3-fluoropicolinic acid

수율 18.0%

반응 조건

후처리

1. 1
   온도upon cooling the material
2. 2
   여과was filtered through celite (4 cm×2 inches)
3. 3
   세척rinsed with H2O (150 mL)
4. 4
   추출extracted with ethyl acetate (2×200 mL)
5. 5
   세척washed with NaCl(sat.)
6. 6
   건조dried over MgSO4
7. 7
   여과filtered
8. 8
   농축concentrated

실험 절차

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.

출처