Hydroxyamine hydrochloride → Ethanone, 1-(6-fluoro-3-pyridinyl)-, oxime
反応式
[F:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=O)[CH3:9])=[CH:4][CH:3]=1.Cl.[NH2:12][OH:13].CC([O-])=O.[Na+]>O.CCO>[F:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=[N:12][OH:13])[CH3:9])=[CH:4][CH:3]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
To a 200-ml, round bottom flask was added, 1-(6-fluoropyridin-3-yl)ethanone (Method 65, 2.5 g, 17.9 mmol), hydroxylamine hydrochloride (2.5 g, 35.8 mmol), and NaOAc (3.7 g, 44.8 mmol) in a solution of water-EtOH (65 ml, 3.3:1). The resulting mixture was heated to 50° C. for 1 hour. The reaction was then allowed to cool to room temperature, partitioned with EtOAc, layers were cut, and organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to afford the title compound in quantitative yield. 1H NMR: 11.49 (s, 1H) 8.47 (s, 1H) 8.17-8.27 (m, 1H) 7.21 (dd, J=8.29, 3.01 Hz, 1H) 2.17 (s, 3H).
後処理
- additionTo a 200-ml, round bottom flask was added
- temperatureto cool to room temperature
- custompartitioned with EtOAc, layers
- dry with materialorganic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-4fe2b9f4f93b454fb72cb30e65a15f56
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08835465B2
反応ノート
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