Reaktion #1797480

ord-959305eaeb8f423aaafc3de2f8b812a8

Reaktionsgleichung

O=C([O-])[O-].[K+].[K+]
potassium carbonate
FC(F)=C(F)OC(F)(F)F
CF3OCF═CF2
CC(F)(F)C(F)(F)C(O)(F)F
Hexafluorobutanol
OCC(F)(F)C(F)C(F)(F)F
CF3CFHCF2CH2OH
FC(C(F)(F)F)C(F)(F)COC(F)(F)C(F)OC(F)(F)F
CF3CFHCF2CH2OCF2CFHOCF3

Lösungsmittel

Reaktionsbedingungen

Temperatur
45°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resulting reaction mixture
  2. 2
    TemperaturThe reactor was cooled
  3. 3
    Filtrationthe contents of the reactor filtered
  4. 4
    Sonstigeto remove the potassium carbonate
  5. 5
    workup.ADDITIONThe resulting product-containing filtrate
  6. 6
    workup.DISTILLATIONwas distilled

Vorschrift

Hexafluorobutanol, CF3CFHCF2CH2OH (65.3 g, 0.34 mol), prepared essentially as described above (Compound 2), was combined with potassium carbonate (9.9 g, 0.072 mol) and 133 g of acetonitrile in a 600 mL Parr reactor. The temperature of the reactor was raised to 45° C. and CF3OCF═CF2 (65.6 g, 0.39 mol) added as a gas over about two hours. The resulting reaction mixture was stirred for about 18 hours at 45° C. The reactor was cooled and the contents of the reactor filtered to remove the potassium carbonate. The resulting product-containing filtrate was distilled using a concentric tube column, with the product cut boiling at 115-119° C. The product structure was confirmed by GCMS.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07790312B2uspto-grants-2010_09