Hydroxyamine hydrochloride → HCID 178471847, 화합물

HRID 2189781노트

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HRID 2189781 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]2

참가 물질

5

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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

  1. waitleft
  2. temperatureto cool overnight
  3. filtrationThe reaction was filtered
  4. washthe residue washed with ethanol
  5. customThe filtrate was evaporated to dryness in vacuo
  6. 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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