Hydrogen Peroxide → 2,4-Dimethylpyridine 1-oxide
反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N:3]=1.[OH:9]O>C(O)(=O)C>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N+:3]=1[O-:9]参加物
4
実験手順
2,4-Dimethylpyridine (40 g, 0.37 mol) was stirred with 30% hydrogen peroxide (170 ml) in glacial acetic acid (400 ml) in an oil bath (80-90° C.) for 24 hr. After cooling to room temperature, the mixture was evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, 1) ether, 2) methanol:chloroform (8:92)) to afford 45 g (98%) of 2,4-dimethyl-pyridine 1-oxide as an oil. 1H NMR (200 MHz, DMSO-d6) δ 2.02 (3H, s), 2.18 (3H, s), 6.69 (1H, d, J=6.5 Hz), 6.82 (1H, s), 7.84 (1H, d, J=6.5 Hz).
後処理
- customthe mixture was evaporated in vacuo
- customthe residue was purified by silica gel column chromatography (eluent, 1) ether, 2) methanol:chloroform (8:92))
出典と根拠
- ORDレコード
- ord-3b557427a55c4199b11e2115640f5a1c
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08106064B2
反応ノート
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