Reaktion #46165

ord-4521dbc84ec14ce1a4ca820a0481d911

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto react for 7 hours at 80° C
  2. 2
    SonstigeEthyl acetate (300 ml) and purified water (200 ml)
  3. 3
    workup.ADDITIONwere further added to the reaction mixture
  4. 4
    ExtraktionThe organic layer extracted with ethyl acetate
  5. 5
    Trocknenwas dried over anhydrous magnesium sulfate
  6. 6
    Einengenconcentrated
  7. 7
    Sonstigethe resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5)

Vorschrift

3′-Hydroxyacetophenone (6.81 g, 50 mmol) and 1-bromo-3-phenyl propane (11.95 g, 60 mmol) were dissolved in dimethylformamide (70 ml). Then, potassium carbonate (15 g) and sodium iodide (0.5 g) were added thereto and the mixture was allowed to react for 7 hours at 80° C. Ethyl acetate (300 ml) and purified water (200 ml) were further added to the reaction mixture prior to stirring for 30 min. The organic layer extracted with ethyl acetate was dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5) to obtain the title compound (12.0 g, yield 94.2%) as a gel.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741323B2uspto-grants-2010_06