반응 #83344

ord-ddb4f227ade34c0fa23ac2005f0389d6

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The solution was concentrated
  2. 2
    workup.ADDITIONethyl acetate added
  3. 3
    세척washed with water
  4. 4
    건조dried over sodium sulfate
  5. 5
    기타the solvent removed
  6. 6
    기타The product was purified by HPLC over silica gel
  7. 7
    세척eluted with 30% ethyl acetate in hexane

실험 절차

2-Chloro-4-phenylquinoline (4.18 mmoles, 10.0 g), 4-aminothiophenol (41.8 mmoles, 5.2 g) and DMAP (41.8 mmoles, 5.0 g) were stirred in 200 ml ethanol and 50 ml THF for 3 days. The solution was concentrated, ethyl acetate added, washed with water, dried over sodium sulfate and the solvent removed. The product was purified by HPLC over silica gel eluted with 30% ethyl acetate in hexane to yield 2-(4-aminophenylthio)-4-phenylquinoline 6.2 g, 45%. Mass Spec (FD) 328. Calculated for C21H16N2S: C, 76.80; H, 4.91 N, 8.53. Found: C, 77.04; H, 5.00; N, 8.55.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05624937uspto-grants-1997_04