Reaktion #93160

ord-9ab274559aec4721905c12d34dea2966

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for three hours
  2. 2
    Filtrationthe precipitated solid was filtered
  3. 3
    WaschenThe product was washed with a small amount of cold acetic acid
  4. 4
    SonstigeIt was dried at 75° C., in vacuo

Vorschrift

A suspension of 274.5 g (2.0 moles) of anthranilic acid, 300 g (2.0 moles) of 4-chloropyridine hydrochloride and 180 g (2.19 moles) of anhydrous sodium acetate in 855 ml of glacial acetic acid was stirred at reflux for three hours. The mixture was cooled to room temperature and the precipitated solid was filtered. The product was washed with a small amount of cold acetic acid followed by cold ether. It was dried at 75° C., in vacuo to give 428 g (85.6%) of 2-(4-pyridinylamino)benzoic acid as the hydrochloride salt, m.p. 275°-280° C.(decompn.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04610991uspto-grants-1986_09