반응 #9278

ord-f014e611ef1f44afbd81fa386b31f468

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added
  2. 2
    온도the mixture was heated
  3. 3
    세척the organic layer was washed with brine
  4. 4
    건조After drying over anhydrous magnesium sulfate and filtration
  5. 5
    농축the solvent was concentrated under reduced pressure
  6. 6
    기타the residue was purified by silica gel column chromatography

실험 절차

After dissolving 7-bromo-2-ethylpyrazolo[1,5-a]pyridine (300 mg) in ethanol (2 mL) and toluene (4 mL), 2,4-dichlorophenylboric acid (508 mg), tetrakis(triphenylphosphine)palladium (0) complex (154 mg) and 2 M aqueous sodium carbonate (1.33 mL) were added and the mixture was heated and stirred at 80° C. for 3 hours under a nitrogen stream. Water was added to the reaction mixture, extraction was performed with ethyl acetate and the organic layer was washed with brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (380 mg) was obtained from the n-hexane:ethyl acetate (100:1) fraction as a light yellow oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091215B2uspto-grants-2006_08