3,4-Dimethylpyridine → 3,4-Dimethylpyridine 1-oxide
反応式
[CH3:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH3:8].C1C=C(Cl)C=C(C(OO)=[O:17])C=1>ClCCl>[CH3:1][C:2]1[CH:3]=[N+:4]([O-:17])[CH:5]=[CH:6][C:7]=1[CH3:8]参加物
4
実験手順
To a solution of 3,4-dimethylpyridine (100.0 g, 0.93 mol) in dichloromethane was added m-CPBA (320.0 g, 1.87 mol) at the room temperature. The reaction mixture was stirred at room temperature overnight, and then quenched with saturated solution of Na2S2O3 (100 mL). The organic layer was separated and the aqueous phase was extracted with CH2Cl2 (300 mL×3). The combined organic layers were dried over anhydrous Na2SO4, filtered and evaporated under vacuum to yield a residue that was purified by column chromatography on silica gel (10-100% MeOH in EtOAc) to give 3,4-dimethylpyridine 1-oxide (70.0 g, 61%).
後処理
- customquenched with saturated solution of Na2S2O3 (100 mL)
- customThe organic layer was separated
- extractionthe aqueous phase was extracted with CH2Cl2 (300 mL×3)
- dry with materialThe combined organic layers were dried over anhydrous Na2SO4
- filtrationfiltered
- customevaporated under vacuum
- customto yield a residue that
- customwas purified by column chromatography on silica gel (10-100% MeOH in EtOAc)
出典と根拠
- ORDレコード
- ord-2c3e9c84d5274d16aad9c3416c7d3d69
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969386B2
反応ノート
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