Reaktion #1165576

ord-0aabdcbbc38d466f976218d0fad2104f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 20 hours
  2. 2
    SonstigeThe solvent was removed under reduced pressure
  3. 3
    workup.DISSOLUTIONthe residue dissolved in dichloromethane (2000 ml)
  4. 4
    ExtraktionThe mixture was extracted with 2M hydrochloric acid
  5. 5
    Extraktionextracted with dichloromethane

Vorschrift

A mixture of N-[1-(4-chlorophenyl)-1-methylethyl]acrylamide (200 g), imidazole (60.9 g), Triton B (20 ml) and 1,4-dioxane (1600 ml) was stirred and boiled under reflux for 20 hours. The solvent was removed under reduced pressure and the residue dissolved in dichloromethane (2000 ml). The mixture was extracted with 2M hydrochloric acid. The combined aqueous extracts were basified with 2M sodium hydroxide solution and extracted with dichloromethane to give N-[1-(4-chlorophenyl)-1-methylethyl]-3-(imidazol-1-yl)propionamide, m.p. 154°-155° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05547972uspto-grants-1996_08