Reaktion #2342

ord-b7642883f03a44b1a3f521f0f19b94b6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITcontinued for 20 hours
  3. 3
    Extraktionthe mixture extracted three times with ethyl acetate
  4. 4
    WaschenThe combined extracts were washed with water and brine
  5. 5
    Trocknendried (MgSO4)
  6. 6
    Sonstigeevaporated
  7. 7
    SonstigeThe residue was triturated with hexane
  8. 8
    Filtrationfiltered

Vorschrift

Sodium hydride (60% dispersion in mineral oil, 0.4 g) was added to a stirred suspension of 4-[4-(4-pyridyl)piperazin-1-yl]phenol (2.55 g) in DMF (25 ml) and the mixture stirred for 20 minutes at room temperature. Allyl chloride (0.756 g) was added dropwise and stirring continued for 20 hours. Ice-water (75 ml) was added and the mixture extracted three times with ethyl acetate. The combined extracts were washed with water and brine, dried (MgSO4) and evaporated. The residue was triturated with hexane and filtered to give 4-[4-(4-pyridyl)piperazin-1-yl]phenol allyl ether (2.5 g) as a solid;

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728701uspto-grants-1998_03