反応 #48594

ord-2eb7446550e549a78eee17324161b795

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture was heated
  2. 2
    温度at reflux overnight
  3. 3
    温度The reaction was cooled
  4. 4
    その他evaporated
  5. 5
    その他then purified by flash column chromatography
  6. 6
    洗浄eluting with 1:9 ethyl acetate/hexane
  7. 7
    workup.ADDITIONthe product containing fractions
  8. 8
    その他evaporated

実験手順

To a solution of benzaldehyde (2 g; 18.9 mmol) and malononitrile (1.37 g; 20.7 mmol) in ethanol (40 ml) was added 5 drops of piperidine and the mixture was heated at reflux overnight. The reaction was cooled, evaporated then purified by flash column chromatography eluting with 1:9 ethyl acetate/hexane and the product containing fractions combined and evaporated to give 930 mg of 2-benzylidene-but-3-yne nitrile.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745638B2uspto-grants-2010_06