Reaktion #2151759

ord-7f4b9e81588e414ebf7187771cd23e0a

Lösungsmittel

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture is refluxed for 4 hours
  2. 2
    Filtrationfiltered through paper
  3. 3
    EinengenThe collected filtrate is concentrated under reduced pressure
  4. 4
    SonstigeThe brown lacquer obtained (340 mg)
  5. 5
    Sonstigeis purified by preparative LC-MS

Vorschrift

389 mg of sodium metabisulphite are added, at a temperature in the region of 20° C., to a solution of 300 mg of 1H-indazole-3-carboxaldehyde and 279 mg of 4,5-dimethyl-1,2-phenylenediamine in 3 ml of dimethylformamide. The reaction mixture is refluxed for 4 hours and then cooled to a temperature in the region of 20° C. and filtered through paper. The collected filtrate is concentrated under reduced pressure. The brown lacquer obtained (340 mg) is purified by preparative LC-MS. 138.8 mg of 5,6-dimethyl-2-(1H-indazol-3-yl)-1H-benzimidazole are thus obtained in the form of a beige-coloured powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08288425B2uspto-grants-2012_10