Reaktion #51442

ord-26d3f179119941d39512cec2ecd01884

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigelowered to −78° C
  2. 2
    Temperaturthe solution is warmed at room temperature
  3. 3
    SonstigeAfter evaporation of the solvent
  4. 4
    workup.DISTILLATIONthe residue is distilled under vacuum

Vorschrift

To a solution of 19 ml (0.135 mole) of diisopropylamine in 125 ml of tetrahydrofuran (THF) cooled at −20° C. is added 80 ml of n-butyllithium (1.6 M in hexane). The temperature is raised to 0° C. for 5 minutes and lowered to −78° C. Then 25 g (0.129 mole) of 2,4-difluoro-bromobenzene is then added and the reaction is stirred at 65° C. for 2 hours. Then, 25 ml (0.164 mole) of hexachloroacetone is added and the solution is warmed at room temperature. After evaporation of the solvent, the residue is distilled under vacuum to give the desired product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06849740B2uspto-grants-2005_02