Reaktion #62863

ord-71c923af91b64034a7eea64cf3aa16cc

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solid which has precipitated
  2. 2
    Sonstigeis isolated
  3. 3
    Sonstigedried

Vorschrift

43 g of 2,5-dichloro-4-methyl-3-nitrobenzoic acid and 108.8 g of Na2S2O4 are boiled in a mixture of 340 ml of glycol monomethyl ether and 340 ml of water for 3 hours. 480 ml of 1/2-concentrated HCl are added to the still warm solution and the mixture is then boiled up once again. After cooling to room temperature, the mixture is poured into 1 l of ice-water and the strongly acid solution is buffered with Na2CO3 (pH 5). The solid which has precipitated is isolated and dried. Melting point: 218°-21°, yield: 32.5 g.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04762844uspto-grants-1988_08