Reaktion #82263

ord-3d0d18ea8fa64a2b90025bea52f01bed

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe solution was refluxed
  2. 2
    Temperaturunder heating for 3 hours
  3. 3
    TemperaturAfter cooling
  4. 4
    workup.DISTILLATIONdistilling off the solvent
  5. 5
    workup.DISSOLUTIONthe resulting residue was dissolved in ethyl acetate
  6. 6
    Waschenwashed with water
  7. 7
    Sonstigedried
  8. 8
    workup.DISTILLATIONAfter distilling off the solvent
  9. 9
    Sonstigethe crystals thus precipitated
  10. 10
    Filtrationwere collected by filtration

Vorschrift

3.42 g of 3,4-diaminobenzonitrile and 4.06 g of ethyl chloroacetoimidate hydrochloride were dissolved in 100 ml of ethanol, and the solution was refluxed under heating for 3 hours. After cooling and distilling off the solvent, the resulting residue was dissolved in ethyl acetate, washed with water, and then dried. After distilling off the solvent, the crystals thus precipitated were collected by filtration to obtain 2.7 g of 2-chloromethyl-5-benzimidazolecarbonitrile.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05620991uspto-grants-1997_04