Hydrazine → HCID 178507285、化合物

HRID 1943905ノート

反応式

HRID 1943905 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=O)[CH2:8][C:9]#[N:10].[NH2:12][NH2:13]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[CH:8]=[C:9]([NH2:10])[NH:13][N:12]=1

参加物

4

反応物 2

HCID 9321HydrazineHCID 115718233-Oxo-3-(pyridin-2-yl)propanenitrile

生成物 1

HCID 178507285HCID 178507285、化合物収率 91%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3-(2-Pyridyl)-3-oxopropanenitrile (3.0 g, 0.37 mol) was dissolved in ethanol (22 mL) and treated with hydrazine (1.9 mL, 0.062 mol) at reflux for 24 hours. The reaction mixture was concentrated, diluted with brine and extracted into ethyl acetate (2×50 mL). The combined organic layers were dried (MgSO4), concentrated and purified by silica gel chromatography eluting with 2-20% methanol in methylene chloride to afford 3-(pyridin-2-yl)-1H-pyrazol-5-amine (3.0 g, 91% yield).

後処理

  1. temperatureat reflux for 24 hours
  2. concentrationThe reaction mixture was concentrated
  3. additiondiluted with brine
  4. extractionextracted into ethyl acetate (2×50 mL)
  5. dry with materialThe combined organic layers were dried (MgSO4)
  6. concentrationconcentrated
  7. custompurified by silica gel chromatography
  8. washeluting with 2-20% methanol in methylene chloride

出典と根拠

ORDレコード
ord-a1636b72dbbb4e759fb21ee6267195f9
出典データセット
uspto-grants-2013_03
特許番号
US08394795B2

反応ノート

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