Reaktion #80045

ord-6b418ab4484245439cbbd6ac784e0b57

Lösungsmittel

Reaktionsbedingungen

Temperatur
137.5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    Filtrationthe solid was collected by filtration
  3. 3
    Waschenwashed with H2O
  4. 4
    SonstigeThe colorless solid was dried under reduced pressure

Vorschrift

To a solution of KOH (6.06 g, 0.11 mol) in 10 mL of H2O was added 40 mL of ethylene glycol and 1-(4-bromophenyl)-cyclopropanecarbonitrile (Intermediate 113, 10.0 g, 0.45 mol). This solution was heated to 135-140° C. for 4 h, cooled to room temperature, and then poured into a mixture of 100 mL ice and 10% aqueous HCl. The resulting mixture was allowed to stand overnight at 5° C., the solid was collected by filtration and washed with H2O. The colorless solid was dried under reduced pressure to give 10.6 g (97%) of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713647B2uspto-grants-2004_03