反应详情

A solution of 24 g (0.22 mol) of 2,3-dimethylpyridine in 100 ml of methylene chloride is treated while cooling with ice with a solution of 46.6 g (0.27 mol) of m-chloroperbenzoic acid in 100 ml of methylene chloride. The reaction mixture is heated under reflux for 2 hours and concentrated in a rotary evaporator. The residue is chromatographed on silica gel with ethyl acetate/methylene chloride (3:1) as the elution agent, the medium pressure flash chromatography method being used and the pressure being produced with nitrogen gas. By recrystallization from ether there is obtained 2,3-dimethylpyridine 1-oxide of melting point 56°.

1. temperatureThe reaction mixture is heated
2. temperatureunder reflux for 2 hours
3. concentrationconcentrated in a rotary evaporator
4. customThe residue is chromatographed on silica gel with ethyl acetate/methylene chloride (3:1) as the elution agent
5. customthe pressure being produced with nitrogen gas
6. customBy recrystallization from ether