Reaktion #1112840

ord-2a9941b2f3ed4116a1c80146c4f64402

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe mixture is washed with a saturated aqueous NaHCO3 solution
  2. 2
    Trocknendried over Na2SO4
  3. 3
    Einengenconcentrated in vacuo
  4. 4
    Sonstigefurther purified by column chromatography (heptane/ethyl acetate=1/1 (v/v), silicagel)

Vorschrift

Part C: 2-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-5-methyl-1H-imidazole-4-carbonyl chloride (1.5 gram, 3.75 mmol), 1-aminopiperidine (0.725 gram, 7.25 mmol) and triethylamine (0.549 gram, 5.44 mmol) are dissolved in dichloromethane and stirred for one hour at room temperature. The mixture is washed with a saturated aqueous NaHCO3 solution, dried over Na2SO4 and concentrated in vacuo and further purified by column chromatography (heptane/ethyl acetate=1/1 (v/v), silicagel) to give 2-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-5-methyl-N-(piperidin-1-yl)-1H-imidazole-4-carboxamide (0.220 gram, 13% yield) as a white foam. MS: 463.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08729101B2uspto-grants-2014_05