反応式
[CH2:1]([C:3]1[C:8]([CH2:9][Cl:10])=[CH:7][CH:6]=[CH:5][N:4]=1)[CH3:2].ClC1C=CC=C(C(OO)=[O:19])C=1>C(Cl)(Cl)Cl>[CH2:1]([C:3]1[C:8]([CH2:9][Cl:10])=[CH:7][CH:6]=[CH:5][N+:4]=1[O-:19])[CH3:2]参加物
4
反応条件
- 温度
- 0 °C
実験手順
The 2-ethyl-3-chloromethylpyridine (2.4 g, 15.4 mmol) was dissolved in CHCl3 (100 mL) and cooled under nitrogen to 0° C. and m-chloroperbenzoic acid (55%, 4.2 g) was added in small portions. The reaction was stirred for 2 hours. The reaction was extracted twice with saturated aqueous sodium bicarbonate (100 mL). The organic phase was dried with MgSO4, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel packed in 98:2 CH2Cl2 :MeOH and eluted with the same. The appropriate fractions were combined and the solvent removed under reduced pressure the give the desired 2-ethyl-3-chloromethylpyridine-N-oxide.
後処理
- extractionThe reaction was extracted twice with saturated aqueous sodium bicarbonate (100 mL)
- dry with materialThe organic phase was dried with MgSO4
- filtrationfiltered
- customthe solvent was removed under reduced pressure
- customThe residue was chromatographed on silica gel
- washMeOH and eluted with the same
- customthe solvent removed under reduced pressure the
出典と根拠
- ORDレコード
- ord-50b5f885709f4236b5aee536d764bea9
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05726172
関連ノート
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