反応 #46167

ord-be4c3fb850964b1bb1e28c3c67e9cbba

反応条件

温度
150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled
  2. 2
    抽出The organic layer was extracted with ethyl acetate
  3. 3
    乾燥dried over anhydrous magnesium sulfate
  4. 4
    濃縮concentrated
  5. 5
    その他the resulting residue was purified by column chromatography (ethyl acetate:hexane=1:3)

実験手順

2-Bromo-3-phenyl-6-(3-phenylpropoxy)indene-1-one (1.0 g, 2.3 mmol) was dissolved in N,N-dimethylformamide (10 ml). Copper (I) cyanide (617 mg, 6.9 mmol) was added thereto and the mixture was stirred for 3 hours at 150° C. The mixture was cooled, and saturated ammonium chloride was added thereto. The organic layer was extracted with ethyl acetate, dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by column chromatography (ethyl acetate:hexane=1:3) to obtain the title compound (700 mg, yield 80%) as a red solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741323B2uspto-grants-2010_06