m-Chloroperbenzoic acid → 6-Methylpyridine-3-carbonitrile 1-oxide
反応式
[CH3:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][N:3]=1.ClC1C=CC=C(C(OO)=[O:18])C=1>ClCCl>[C:6]([C:5]1[CH:8]=[CH:9][C:2]([CH3:1])=[N+:3]([O-:18])[CH:4]=1)#[N:7]参加物
4
実験手順
A mixture of 6-methylnicotinonitrile (4.15 g) and 3-chloroperbenzoic acid (8.3 g) in dichloromethane (200 ml) was stirred under an argon atomosphere at room temperature for 16h. The dichloromethane was evaporated under reduced pressure and the residue purified by flash column chromatography on silica (K60), using ethyl acetate and then methanol: dichloromethane (1:9 by volume) as eluting solvent to give 5-cyano-2-methylpyridine-1-oxide, mp 133.5°.
後処理
- customThe dichloromethane was evaporated under reduced pressure
- customthe residue purified by flash column chromatography on silica (K60)
- washmethanol: dichloromethane (1:9 by volume) as eluting solvent
出典と根拠
- ORDレコード
- ord-a78378da87434bf7a8573388e582ea7e
- 出典データセット
- uspto-grants-1991_03
- 特許番号
- US04999364
反応ノート
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