반응 #46154

ord-9f1d80b364074f929dd880780932bf51

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with saturated ammonium chloride
  2. 2
    기타The organic layer obtained
  3. 3
    추출by extracting the reaction mixture with ethyl acetate
  4. 4
    건조was dried over anhydrous magnesium sulfate
  5. 5
    농축concentrated
  6. 6
    기타the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:4)

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741323B2uspto-grants-2010_06