Hydroxylamine → HCID 53396275、化合物
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=O)[CH3:9])=[CH:4][CH:3]=1.[NH2:11][OH:12].O>C(O)(=O)C.O1CCOCC1.C(Cl)(Cl)Cl.C(O)(C)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8](=[N:11][OH:12])[CH3:9])=[CH:4][CH:3]=1参加物
7
反応条件
- 温度
- 150 °C
実験手順
Combine 1-(6-chloropyridin-3-yl)ethanone (3.4 g, 22.8 mmol), hydroxylamine (50%) in water (5.77 g, 87.4 mmol) and 0.75 mL of acetic acid in 15 mL of dioxane in a pressure vessel. Seal the vessel and heat the mixture in an oil bath for 3 h at 150° C. Cool the mixture to RT. Dilute with chloroform/IPA (3/1), wash with water, and aqueous saturated sodium chloride. Separate the layers and dry the organic layer over sodium sulfate. Concentrate in vacuo to afford the title compound (3.52 g, 94%). MS (ES) m/z 171 [M+1]+.
後処理
- customSeal the vessel
- temperatureCool the mixture to RT
- washwash with water, and aqueous saturated sodium chloride
- customSeparate the layers
- dry with materialdry the organic layer over sodium sulfate
- concentrationConcentrate in vacuo
出典と根拠
- ORDレコード
- ord-f8fc75ea881242f49d7b4f0ec095152f
- 出典データセット
- uspto-grants-2012_02
- 特許番号
- US08114872B2
反応ノート
読み込み中…