Hydrazinium bromide → 1160227-03-1

HRID 75508

반응식

HRID 75508 반응식
O=[C:2]([CH3:12])[CH:3]([C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1)[C:4]#[N:5].Br.[NH2:14][NH2:15]>CCO.O>[CH3:12][C:2]1[NH:15][N:14]=[C:4]([NH2:5])[C:3]=1[C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1

참가 물질

5

반응물 2

HCID 159693Hydrazinium bromideHCID 673626493-Oxo-2-(pyridin-3-yl)butanenitrile

생성물 1

HCID 673636361160227-03-1

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

3-Oxo-2-pyridin-3-yl-butyronitrile (step 1) (1.00 g, 6.49 mmol) was dissolved in EtOH (10 ml) and water (2 ml). Hydrazine hydrobromide (2.82 g, 24.97 mmol) was added and the reaction mixture was heated at reflux for 1 hour. The solvent was removed in vacuo and the residue was partitioned between EtOAc and sat. NaHCO3. The organic phase was washed with water and brine, dried (MgSO4), filtered and the solvent was removed in vacuo to afford the title compound which was used without further purification; 1H NMR (d6-DMSO, 400 MHz) δ 11.51 (1H, br), 8.60 m), 8.40 (1H, m), 7.72 (1 h, m), 7.39 (1H, m), 4.60 (2H, br), 2.19 (3H, s).

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 1 hour
  3. customThe solvent was removed in vacuo
  4. customthe residue was partitioned between EtOAc and sat. NaHCO3
  5. washThe organic phase was washed with water and brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-50f9fa1b87994be683590f893a48119e
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835444B2

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