Reaktion #1445884

ord-c498807fa1ea4e88ac9ab9ba21af462a

Reagenzien

Keine

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Temperaturthe resulting mixture was heated
  3. 3
    SonstigeThe solvent was evaporated under vacuum
  4. 4
    workup.DISSOLUTIONthe resulting oil was dissolved in methylene chloride (2 mL)
  5. 5
    Filtrationfiltered through silica gel (2:1 EtOA/hexane)
  6. 6
    SonstigeThe solvent was evaporated under vacuum

Vorschrift

To a mixture of 2-phenylbenzimidazole (1.02 g, 5.25 mmol) in DMC (10 mL), DBU (0.80 g, 5.25 mmol) was added and the resulting mixture was heated to reflux (90° C.) for 6 hours. The solvent was evaporated under vacuum and the resulting oil was dissolved in methylene chloride (2 mL) and filtered through silica gel (2:1 EtOA/hexane). The solvent was evaporated under vacuum to afford 1-methyl-2-phenylbenzimidazole as a solid. The yield of 1-methyl-2-phenylbenzimidazole as determined by HPLC analysis was 98%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06596877B2uspto-grants-2003_07