Reaktion #523783

ord-890635a35dfe40ce913a0d17b80ad267

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 10 hours
  3. 3
    TemperaturAfter cooling
  4. 4
    Waschenthe reaction mixture was washed with water
  5. 5
    Trocknendried over sodium sulfate
  6. 6
    Sonstigeevaporated under reduced pressure
  7. 7
    SonstigeThe residue was triturated with ether
  8. 8
    Temperaturcooled
  9. 9
    Filtrationfiltered

Vorschrift

A mixture of 1.5 g of 2-allyl-4-fluorophenol, 3.1 g of 8-(3-chloropropyl)-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, 0.7 g of potassium carbonate and 40 ml of toluene was heated under reflux for 10 hours. After cooling, the reaction mixture was washed with water, dried over sodium sulfate and evaporated under reduced pressure. The residue was triturated with ether, cooled and filtered to give 8-{3-(2-allyl-4-fluorophenoxy)propyl}-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, m.p. 110° - 113° C; recrystallized from cyclohexane, m.p. 117° - 117.5° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04009275uspto-grants-1977_02