Reaktion #55657

ord-f293bf93d94348b09e6e14922f208abc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA mixture of 9.23 g
  2. 2
    workup.ADDITIONthe mixture is poured onto 100 ml
  3. 3
    ExtraktionThe aqueous phase is extracted with 2×75 ml
  4. 4
    Waschenwashed with distilled water until chloride-free
  5. 5
    Trocknendried over anhydrous magnesium sulphate
  6. 6
    Filtrationfiltered
  7. 7
    Sonstigeevaporated in vacuo

Vorschrift

A mixture of 9.23 g. of 3-nitro-4-chloro-benzophenone, 10 ml. of ethanol and 10.3 g. of N-methyl-N-octylamine is stirred at 80° to 85° C. for 30 minutes, and then the mixture is poured onto 100 ml. of ice water. The aqueous phase is extracted with 2×75 ml. of benzene. The benzene phases are combined, washed with distilled water until chloride-free, dried over anhydrous magnesium sulphate, filtered, and evaporated in vacuo. 11.57 g. of 3-nitro-4-(N-methyl-N-octylamino)-benzophenone are obtained in the form of an oily residue. On the basis of thin layer chromatographical examination, a pure, uniform product is obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04221739uspto-grants-1980_09