1-(6-Chloropyridin-3-yl)butan-1-ol → 1-(6-Chloropyridin-3-yl)butan-1-one
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH:8]([OH:12])[CH2:9][CH2:10][CH3:11])=[CH:4][CH:3]=1.[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>ClCCl>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=[O:12])[CH2:9][CH2:10][CH3:11])=[CH:4][CH:3]=1参加物
4
実験手順
To a solution of 1-(6-chloropyridin-3-yl)butan-1-ol (210 mg, 1.13 mmol) in 10 mL dichloromethane was added 2 g of silica gel, followed by pyridinium chlorochromate (488 mg, 2.26 mmol) The mixture was stirred at room temperature 5 h. The mixture was filtered through a plug of silica gel, eluting with 100 mL dichloromethane. The eluent was concentrated to give 1-(6-chloropyridin-3-yl)butan-1-one (210 mg). 1H NMR (400 MHz, CDCl3) δ 8.88-8.96 (m, 1H), 8.14-8.20 (m, 1H), 7.42 (d, J=8.4 Hz, 1H), 2.92 (t, J=7.2 Hz, 2H), 1.70-1.82 (m, 2H), 0.99 (t, J=7.4 Hz, 3H).
後処理
- filtrationThe mixture was filtered through a plug of silica gel
- washeluting with 100 mL dichloromethane
- concentrationThe eluent was concentrated
出典と根拠
- ORDレコード
- ord-cd6474f53fc24401aef73a8f4f839241
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859591B2
反応ノート
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