2,3-Lutidine → Pyridine, 2,3-dimethyl-, 1-oxide
反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N:3]=1.ClC1C=CC=C(C(OO)=[O:17])C=1>C(Cl)Cl>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:17]参加物
4
実験手順
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°.
後処理
- temperatureThe reaction mixture is heated
- temperatureunder reflux for 2 hours
- concentrationconcentrated in a rotary evaporator
- customThe residue is chromatographed on silica gel with ethyl acetate/methylene chloride (3:1) as the elution agent
- customthe pressure being produced with nitrogen gas
- customBy recrystallization from ether
出典と根拠
- ORDレコード
- ord-39749d82d8984a9b830f19e45fb8b4be
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04766133
反応ノート
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