Hydrochloric Acid → 2-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)ethan-1-ol

HRID 75581

反応式

HRID 75581 の反応式
[CH3:1][C:2]([CH3:9])([CH3:8])[C:3](=O)[CH2:4][C:5]#[N:6].Cl.[NH:11]([CH2:13][CH2:14][OH:15])[NH2:12]>C(O)C>[NH2:6][C:5]1[N:11]([CH2:13][CH2:14][OH:15])[N:12]=[C:3]([C:2]([CH3:9])([CH3:8])[CH3:1])[CH:4]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 80172-HydrazinoethanolHCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-

生成物 1

HCID 162278772-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)ethan-1-ol収率 97.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 4,4-dimethyl-3-oxo-pentanenitrile (5.00 g, 40.0 mmol), concentrated HCl (0.1 mL), and 2-hydrazino ethanol (2.98 mL, 44.0 mmol) in ethanol (40 mL) was refluxed for 20 h. The reaction mixture was then concentrated in vacuo. The resulting oily solid was washed with cyclohexane (30 mL), and dissolved in MeOH (5 mL) and H2O (5 mL) and lyophilised to give the title compound as a white powder (7.13 g, 97%). LCMS (Method 3): Rt 0.43 min, m/z 184 [MH+].

後処理

  1. concentrationThe reaction mixture was then concentrated in vacuo
  2. washThe resulting oily solid was washed with cyclohexane (30 mL)
  3. dissolutiondissolved in MeOH (5 mL)

出典と根拠

ORDレコード
ord-2de6a3d9b2ca4b78bda6fb2329a4e94d
出典データセット
uspto-grants-2014_09
特許番号
US08835431B2

関連ノート

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