m-Chloroperbenzoic acid → 2-Chloro-4-methylpyridine 1-oxide
反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[Cl:12][C:13]1[CH:18]=[C:17]([CH3:19])[CH:16]=[CH:15][N:14]=1>C(Cl)(Cl)Cl>[Cl:12][C:13]1[CH:18]=[C:17]([CH3:19])[CH:16]=[CH:15][N+:14]=1[O-:9]参加物
4
実験手順
40% meta-chloroperbenzoic acid (13.5 g, 31.4 mmol) was added at ambient temperature to a solution of 2-chloro-4-methyl-pyridine (2.0 g, 1.5 mmol) in chloroform (20 mL) and heated at reflux for 24 h. After allowing to cool, the mixture was washed with water followed by sodium bicarbonate solution. The separated organic phase was further washed with water and brine, dried over anhydrous sodium sulfate and concentrated to give a residue which was purified by column chromatography over silica gel (60-120 mesh) using 10% methanol in ethyl acetate as eluent to afford 2-chloro-4-methyl-pyridine 1-oxide (1.0 g, 45%) as a deep brown oily liquid.
後処理
- temperatureheated
- temperatureat reflux for 24 h
- temperatureto cool
- washthe mixture was washed with water
- washThe separated organic phase was further washed with water and brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customto give a residue which
- customwas purified by column chromatography over silica gel (60-120 mesh)
出典と根拠
- ORDレコード
- ord-c2ddec53bd744cd7b5a933c42f3d5d64
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524705B2
反応ノート
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