反応 #46154

ord-9f1d80b364074f929dd880780932bf51

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with saturated ammonium chloride
  2. 2
    その他The organic layer obtained
  3. 3
    抽出by extracting the reaction mixture with ethyl acetate
  4. 4
    乾燥was dried over anhydrous magnesium sulfate
  5. 5
    濃縮concentrated
  6. 6
    その他the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:4)

実験手順

6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylate ethyl ester (2 g, 6.80 mmol), potassium carbonate (1.41 g, 10.194 mmol), and sodium iodide (200 mg, 1.359 mmol) were dissolved in dimethylformamide (100 ml). 1-Bromo-3-phenylpropane (2.01 ml, 13.59 mmol) was added thereto at room temperature, was stirred for 12 hours at 60° C., and washed with saturated ammonium chloride. The organic layer obtained by extracting the reaction mixture with ethyl acetate was dried over anhydrous magnesium sulfate, concentrated, and the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:4) to obtain the title compound (yield 85%) as a dark red solid.

出典

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