Reaktion #5854

ord-da0c1141ff4a4a2e80f2daaa6a47cc27

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe thus-formed mixture was then refluxed
  2. 2
    Temperaturunder heating for 10 hours
  3. 3
    Temperaturto cool
  4. 4
    Sonstigethe insoluble substance was removed by filtration
  5. 5
    WaschenThe thus-obtained filtrate was washed with water
  6. 6
    Einengenthe concentrated for the purpose
  7. 7
    Sonstigeof recovering the solvent
  8. 8
    Sonstigeto obtain a slightly brown powder
  9. 9
    SonstigeThe powder was then recrystallized from acetone

Vorschrift

11.4 g (0.03 mole) of N,N'-bis-(2,6-diisopropylphenyl) guanidine, 8.7 g (0.03 mole) of α,α-dibromo-p-xylene and 2.1 g (0.015 mole) of anhydrous potassium carbonate were added to 50 ml of toluene. The thus-formed mixture was then refluxed under heating for 10 hours. After the mixture had been allowed to cool, the insoluble substance was removed by filtration. The thus-obtained filtrate was washed with water and the concentrated for the purpose of recovering the solvent to obtain a slightly brown powder. The powder was then recrystallized from acetone to obtain 6.6 g of white powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05246810uspto-grants-1993_09