Reaktion #2068462

ord-adf91562ba9149e5bf929ccc7504786b

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONThe excess thionyl chloride was distilled off
  2. 2
    ExtraktionThe product was extracted with methylene chloride
  3. 3
    SonstigeFor purification
  4. 4
    Sonstigethe product was recrystallized

Vorschrift

36.5 mmoles of 4-(4-pentyl-1-bicyclo(2,2,2)-octyl)-benzoic acid were refluxed with 50 ml of thionyl chloride for 1 hour. The excess thionyl chloride was distilled off. The resulting acid chloride was added dropwise to a solution of 36.5 mmoles of 2,3-dicyano-4-pentylphenol in 100 ml of pyridine. The reaction mixture was stirred at 80° C. until the reaction had ended and was then poured onto dilute hydrochloric acid. The product was extracted with methylene chloride. For purification, the product was recrystallized. It displays an enantiotropic nematic phase (K 130.9 N (137.9) I) and has a negative DCA.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04514317uspto-grants-1985_04