m-Chloroperbenzoic acid → 3-cyclohexyl-2-methylpyridine N-oxide
反応式
[CH:1]1([C:7]2[C:8]([CH3:13])=[N:9][CH:10]=[CH:11][CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1C=C(Cl)C=C(C(OO)=[O:22])C=1>C(Cl)Cl>[CH:1]1([C:7]2[C:8]([CH3:13])=[N+:9]([O-:22])[CH:10]=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1参加物
4
実験手順
A solution of 3-cyclohexyl-2-methylpyridine (170 mg, 1.0 mmol), in CH2Cl2 (5 mL) was treated with MCPBA (0.33 g, 1.9 mmol) for 18 hours. The solution was then washed with saturated NaHCO3 solution (5 mL), the phases separated, and the aqueous extracted with CH2Cl2 (2×10 mL). The combined organic phases were then dried (Na2SO4), filtered, and concentrated to afford crude 3-cyclohexyl-2-methylpyridine N-oxide as a white solid (0.215 g) which was used immediately in the next reaction.
後処理
- washThe solution was then washed with saturated NaHCO3 solution (5 mL)
- customthe phases separated
- extractionthe aqueous extracted with CH2Cl2 (2×10 mL)
- dry with materialThe combined organic phases were then dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-f2ae57fe4c34450fb80930496f553237
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07291631B2
反応ノート
読み込み中…