Reaktion #364656

ord-643ea3ad26fb47a3a47d07f0af50bc60

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was heated
  2. 2
    Temperaturunder reflux for 1 hour
  3. 3
    EinengenThe reaction mixture was concentrated to dryness
  4. 4
    workup.DISSOLUTIONThe resultant residue was dissolved in ethyl acetate
  5. 5
    Waschenthe solution was washed with water
  6. 6
    Sonstigedried
  7. 7
    SonstigeAfter evaporation of the solvent
  8. 8
    Sonstigethe residue was purified by column chromatography on silica gel

Vorschrift

To a solution of ethyl 2-chloro-1-[(2′-cyanobiphenyl-4-yl)methyl]benzimidazole-7-carboxylate (1.0 g) in ethanol (30 ml) was added NaOEt (0.17 g) and the mixture was heated under reflux for 1 hour. The reaction mixture was concentrated to dryness. The resultant residue was dissolved in ethyl acetate and the solution was washed with water, and then dried. After evaporation of the solvent, the residue was purified by column chromatography on silica gel to give the title compound as colorless crystals(0.37 g, 70%). 1H-NMR and IR spectra indicate that the product according to this working Example is completely identical with that obtained in Working Example 4.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06355808B2uspto-grants-2002_03