Reaktion #446822

ord-9fbc043d628d4fb7a32acc12cee0b1e0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter the end of the addition the agitation
  2. 2
    Sonstigeat 70° C
  3. 3
    TemperaturThe reaction mixture is cooled
  4. 4
    SonstigeThe expected product crystallizes
  5. 5
    Sonstigeis separated by filtration
  6. 6
    SonstigeAfter drying it
  7. 7
    Sonstigeis recrystallized from ethanol

Vorschrift

A mixture comprising 0.18 mole (50 g) of 2,4-dinitro 1,3,5-trichlorobenzene and 250 ml of dioxane are heated at 70° C. 0.64 mole (219.9 g) of sodium ethylate in solution at a concentration of 20% in ethanol are then added while agitating. After the end of the addition the agitation is continued two more hours at 70° C. The reaction mixture is cooled and diluted with iced water. The expected product crystallizes and is separated by filtration. After drying it is recrystallized from ethanol. It melts at 105° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05002585uspto-grants-1991_03