反応 #461704

ord-300e27b72f9f454b8b8e4098d4c2d88f

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate
  2. 2
    抽出The organic extract
  3. 3
    洗浄is washed sequentially with saturated sodium hydrogen carbonate solution and brine
  4. 4
    乾燥dried over MgSO4
  5. 5
    濃縮concentrated in vacuo
  6. 6
    その他to obtain an orange solid
  7. 7
    その他Dry column chromatography of the solid

実験手順

β-[(Formylmethyl)amino]-2-benzofuranacrylonitrile (1.00 g, 3.33 mmol) is added dropwise to trifluoroacetic acid (5 mL). The reaction mixture is stirred at room temperature for one hour, diluted with water and extracted with ethyl acetate. The organic extract is washed sequentially with saturated sodium hydrogen carbonate solution and brine, dried over MgSO4, decolorized with charcoal and concentrated in vacuo to obtain an orange solid. Dry column chromatography of the solid using silica gel and methylene chloride gives the title product as a brown-white solid (0.32 g 46% mp 157°-160.5° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05480902uspto-grants-1996_01