Reaktion #523205

ord-d6fb7cb9aaa545c588b13cf3922d0302

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat a reaction temperature of 175° C
  2. 2
    WaschenThe reaction product was washed
  3. 3
    Sonstigedried as before

Vorschrift

750 g of p-nitrotoluene was oxidized in 2250 ml of glacial acetic acid, after the addition of 15 g of NH4Br, 4.5 g of Co(OAc)2 . 4H2O and 4.5 g of Mn(OAc)2 . 4H2O, at a reaction temperature of 175° C. The reaction product was washed and dried as before. 795 g (87% of the theory) of brown-discolored p-nitrobenzoic acid was obtained, having a melting point of 235°-36° C. The solution of 1 g of the product in 10 g of dimethylsulfoxide has a value of 40 on the iodine color scale. After recrystallization three times from glacial acetic acid, the melting point was 237°-40° C, while the iodine number remained unchanged.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04007223uspto-grants-1977_02