Hydrogen Peroxide → 2,6-Dichloropyridine N-Oxide

Participants

Reaction Steps

After the reaction solution of trifluoroacetic acid (485 mL, 6.3 mol), 2,6-dichloropyridine (48 g, 324 mmol) and 35% hydrogen peroxide (85.0 mL, 971 mmol) was stirred for 6.5 h under the condition of reflux, it was cooled to room temperature. The reaction solution was poured into beaker contained 2.4 L water, and cooled overnight at 0° C. The solid (unreacted 2,6-dichloropyridine) was removed through a suction filtration. The filtrate was concentrated, to which 500 mL chloroform was added, and potassium carbonate was added until no gas was produced. It was filtrated. The filtrate was concentrated under vacuum to afford 46.6 g light yellow solid, 87.6%.

Provenance & Evidence