反应详情

To a stirring solution of 4-difluoromethylpyridine (5.00 g, 38.7 mmol) in CH2Cl2 (77 mL, 0.5 M) at 0° C. was added 77% meta-chloroperbenzoic acid (10.7 g, 46.5 mmol) and the ice bath was removed and stirring continued for 20.5 hr. The reaction mixture was concentrated to dryness and reaction residue purified by flash column chromatography (100:0-95:5 CH2Cl2/MeOH) to afford 4-difluoromethyl-pyridine-N-oxide as a colorless solid (5.62 g, >99%); 1H NMR (400 MHz, CDCl3) δ 8.26 (d, J=6.4 Hz, 2H), 7.40 (d, J=6.4 Hz, 2H), 6.63 (t, J=55.7 Hz, 1H).

1. customthe ice bath was removed
2. concentrationThe reaction mixture was concentrated to dryness and reaction residue
3. custompurified by flash column chromatography (100:0-95:5 CH2Cl2/MeOH)