Hydrazinium bromide → 1160227-03-1

HRID 75508

反応式

HRID 75508 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 673636361160227-03-1

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-50f9fa1b87994be683590f893a48119e
出典データセット
uspto-grants-2014_09
特許番号
US08835444B2

関連ノート

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