Reaktion #415821

ord-98e3ef4685bc4e8fb9ab499c88062115

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux temperature for 15 hours
  2. 2
    SonstigeThereafter, the solvent is evaporated under reduced pressure
  3. 3
    Sonstigethe residue triturated in 4-methyl-2-pentanone
  4. 4
    FiltrationThe solid is recovered by filtration
  5. 5
    Sonstigecrystallized from acetonitrile

Vorschrift

In a manner similar to that previously described, 4.2 parts of 1-[2,4-dichloro-β-(2,4-dichlorobenzyloxy)phenethyl]imidazole, 1.7 parts of 2-chloro-4'-fluoroacetophenone and 40 parts of methylene chloride are mixed together and stirred at reflux temperature for 15 hours. Thereafter, the solvent is evaporated under reduced pressure and the residue triturated in 4-methyl-2-pentanone. The solid is recovered by filtration and crystallized from acetonitrile to obtain a purified 1-[2,4-dichloroβ-(2,4-dichlorobenzyloxy)phenethyl]-3-(p-fluorobenzoylmethyl)imidazolium chloride product, m.p. 181° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04017631uspto-grants-1977_04