Reaktion #92931

ord-8104772c20514b93bc2857cc39bb66e2

Reaktionsgleichung

CC(C)(Br)C(=O)c1ccccc1
α-bromoisobutyrophenone
Cn1ccnc1
1-methylimidazole
C[NH+]1C=CN(C(C)(C)C(=O)c2ccccc2)C1.[Br-]
1-methyl-3-(1,1-dimethyl-2-phenyl-2-oxoethyl)-1H-imidazolium bromide
Ausbeute 63.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was decanted
  2. 2
    SonstigeThe solvent was again decanted
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in acetonitrile
  4. 4
    workup.ADDITIONto adding a small portion of ethyl acetate
  5. 5
    FiltrationA white precipitate was collected by filtration
  6. 6
    Sonstigerecrystallized from methanol/ethyl acetate

Vorschrift

A solution of 4.6 g (0.02 mol) of α-bromoisobutyrophenone and 1.8 g (0.022 mol) of 1-methylimidazole in 30 ml of diethyl ether was stirred at room temperature for approximately 48 hours. The solvent was decanted and the resulting oil was slurried in ethyl acetate. The solvent was again decanted and the residue was dissolved in acetonitrile prior to adding a small portion of ethyl acetate. A white precipitate was collected by filtration and recrystallized from methanol/ethyl acetate to afford 3.88 g of 1-methyl-3-(1,1-dimethyl-2-phenyl-2-oxoethyl)-1H-imidazolium bromide as glittering white flakes. (63% yield) mp=137°-140° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04609670uspto-grants-1986_09