Reaktion #83181

ord-ca88297e1e8d45faa969928145c45ee2

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas cooled to room temperature
  2. 2
    ExtraktionThe product was extracted with ethylene dichloride
  3. 3
    Waschenthen washed with water
  4. 4
    Trocknendried over magnesium sulfate
  5. 5
    EinengenThe solvent was concentrated

Vorschrift

To a 500 mL flask was charged 75.0 g (0.24 mole) of alpha-n-butyl-alpha-(4-chlorophenyl)-1H-1,2,4-triazole-1-propanenitrile followed by 300 mL of 95% sulfuric acid. The mixture was stirred at 90° C. for 7 days after which the mixture was cooled to room temperature, diluted with ice and neutralized with ammonium hydroxide until basic (pH 8). The product was extracted with ethylene dichloride then washed with water and dried over magnesium sulfate. The solvent was concentrated and gave 45 g (56.5% yield) of a solid melting point 197°-199° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05624916uspto-grants-1997_04