반응 #92931

ord-8104772c20514b93bc2857cc39bb66e2

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was decanted
  2. 2
    기타The 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
    여과A white precipitate was collected by filtration
  6. 6
    기타recrystallized from methanol/ethyl acetate

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04609670uspto-grants-1986_09