Reaktion #1698012

ord-64bd67555037490aa52e01b9bdbd3d3d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture is refluxed for 30 minutes
  2. 2
    Extraktionextracted with dichlormethane
  3. 3
    TrocknenThe organic phases are dried over magnesium sulfate
  4. 4
    Sonstigethe solvent is evaporated under vacuum

Vorschrift

30 ml (150 mmol) of hydrogen chloride-solution (5 M in water) and 1.5 ml (14.68 mmol) 2,4-Pentandione are added to a solution of (7.34 mmol) of 2-Amino-3,5-dimethylphenylamine (example X, Step 1) in 112 ml ethanol. The reaction mixture is refluxed for 30 minutes. The solution is neutralized with saturated sodium hydrogen carbonate solution (to pH 7) and extracted with dichlormethane. The organic phases are dried over magnesium sulfate and the solvent is evaporated under vacuum to afford 2,5,7-Trimethyl-1H-benzimidazole (1.46 g) in quantitative yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06984646B2uspto-grants-2006_01