Hydroxylamine → HCID 53396275, 화합물
반응식
[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]=1참가 물질
7
반응 조건
- 온도
- 150 °C
실험 절차
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]+.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f8fc75ea881242f49d7b4f0ec095152f
- 출처 데이터셋
- uspto-grants-2012_02
- 특허 번호
- US08114872B2
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