반응 #653031

ord-8cca7be01d00488789d78e7431a7d9c8

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was refluxed for 14 hours
  2. 2
    온도The reaction mixture was cooled to room temperature
  3. 3
    기타The organic layer was separated
  4. 4
    건조dried with anhydrous sodium sulfate
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The residue was separated
  7. 7
    기타purified with column chromatography (ethyl acetate/toluene=1/10)

실험 절차

Under argon atmosphere, a mixture of 7-(trifluoromethanesulfoxy)-1-tetralone (17.5 g), 4-fluorophenyl borate (10.0 g), potassium carbonate (16.6 g), toluene (500 ml), ethanol (50 ml) and water (50 ml) was stirred at room temperature for 30 minutes, and to the mixture was added tetrakis(triphenylphosphine)palladium (2.08 g). The mixture was refluxed for 14 hours. The reaction mixture was cooled to room temperature. The organic layer was separated, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/toluene=1/10) to give 7-(4-fluorophenyl)-1-tetralone (13.8 g) as brown oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06172061B2uspto-grants-2001_01