Reaction #415821

ord-98e3ef4685bc4e8fb9ab499c88062115

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

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

Procedure

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.

Source

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