반응 #804273

ord-e1c5511e683f41ea9684beca2c6ba8ea

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타degassed with N2
  2. 2
    기타The reaction mixtures
  3. 3
    기타were irradiated
  4. 4
    기타a microwave (300 W, 180° C., 30 min)
  5. 5
    기타The reaction mixtures
  6. 6
    여과the resulting precipitate was filtered
  7. 7
    세척washed with DMF and water
  8. 8
    기타dried

실험 절차

3-(4-Bromo-phenyl)-5-methyl-2H-isoquinolin-1-one (200 mg, 0.64 mmol), zinc cyanide (90 mg, 0.76 mmol) and tetrakis(triphenylphosphine)palladium(0) (74 mg, 0.064 mmol) were stirred in DMF (2.1 mL) and degassed with N2. The reaction mixtures were irradiated using a microwave (300 W, 180° C., 30 min). The reaction mixtures were combined and the resulting precipitate was filtered, washed with DMF and water and dried to give 4-(5-methyl-1-oxo-1,2-dihydro-isoquinolin-3-yl)-benzonitrile as a yellowish solid (718 mg, 79%) which was used in the next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09193689B2uspto-grants-2015_11