Hydroxyamine hydrochloride → HCID 178471847, 화합물
반응식
[C:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:7]=[CH:6]2)#[N:2].C(=O)(O)[O-].[Na+].Cl.[NH2:25][OH:26]>C(O)C>[OH:26][NH:25][C:1](=[NH:2])[C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:7]=[CH:6]2참가 물질
5
반응 조건
- 온도
- 50 °C
실험 절차
Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate (D47) (3.84 g, 15.8 mmol) was dissolved in ethanol (100 ml) and sodium bicarbonate (6.6 g, 79 mmol) and then hydroxylamine hydrochloride (3.3 g, 47.4 mmol) were added. The reaction was heated to 50° C. for a total of 11 hours and then left to cool overnight. The reaction was filtered and the residue washed with ethanol. The filtrate was evaporated to dryness in vacuo and the resultant solid triturated with ether to generate the title compound (3.79 g) as a white solid. MS (ES): C13H16N4O3 requires 276; found (MH+) 277.
후처리
- waitleft
- temperatureto cool overnight
- filtrationThe reaction was filtered
- washthe residue washed with ethanol
- customThe filtrate was evaporated to dryness in vacuo
- customthe resultant solid triturated with ether
출처 및 근거
- ORD 기록
- ord-799d95a2309f4ed4acc65eada05d0b08
- 출처 데이터셋
- uspto-grants-2012_12
- 특허 번호
- US08324254B2
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