Reaktion #76821

ord-83f8d50e146b4a3ebdf0a609467648ec

Reagenzien

Reaktionsbedingungen

Temperatur
55°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter the exothermic reaction
  2. 2
    workup.DISTILLATIONThe reaction mixture was then distilled
  3. 3
    Sonstigeof less then 80° C. was collected
  4. 4
    WaschenThis fraction was washed with an aqueous HCl solution
  5. 5
    workup.DISTILLATIONdistilled over conc. H2SO4

Vorschrift

A solution of (CF3)2CFOCF2CF2I (21.3 g) in isopropanol (8 mL) was added dropwise to a suspension of Al chips (1 g) and HgCl2 (0.4 g) in isopropanol (30 mL). After the exothermic reaction was completed, the reaction mixture was stirred for 1 hour at 55° C. The reaction mixture was then distilled and a fraction with a b.p. of less then 80° C. was collected. This fraction was washed with an aqueous HCl solution and then distilled over conc. H2SO4 to give (CF3)2CFOCF2CHF2 (11.8 g, 80% yield), b.p. 44 to 46° C. The 1H and 19F NMR were in accord with the assigned structure:

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06703533B1uspto-grants-2004_03