Reaktion #220157

Reaktionsgleichung

C3F7OCFHCF2OC2H4OH

potassium carbonate

Hexafluoropropene

C3F7OCFHCF2OC2H4OH

→

C3F7OCHFCF2OC2H4OCF2CFHCF3

Ausbeute 86.3%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto give a 106.3 g fractionation cut
2. 2
   SonstigeThe reactor was sealed
3. 3
   TemperaturThe reactor was cooled
4. 4
   Filtrationthe contents filtered into a 1-L separatory funnel
5. 5
   Waschenwater washed four times
6. 6
   Trocknendried with anhydrous sodium sulfate
7. 7
   Filtrationfiltered
8. 8
   Waschenwashed
9. 9
   Trocknendried with anhydrous sodium sulfate
10. 10
    Filtrationfiltered

Vorschrift

Perfluoropropylvinyl ether (139.0 g, 0.52 mole), potassium carbonate (19.3 g, 0.14 mole), ethylene glycol (155.5 g, 2.5 mole) and acetonitrile (200 mL) were combined in a 600 mL Parr reactor. The reactor was sealed and heated to 30° C. for 2.75 hours. The reaction mixture was filtered and then water washed four times to give 146.4 g of C3F7OCFHCF2OC2H4OH (54.2%) and (C3F7OCFHCF2OCH2)2 (43.4%). This material was combined with 179 g from a previous run consisting of 21.6% C3F7OCFHCF2OC2H4OH and 76.1% (C3F7OCFHCF2OCH2)2 and fractionated to give a 106.3 g fractionation cut boiling from 167-173° C. of C3F7OCFHCF2OC2H4OH (80.8% pure). This material along with potassium carbonate (7.3 g, 0.052 mole) and acetonitrile (200 mL) were added to a 600 mL Parr reactor. The reactor was sealed and heated to 30° C. Hexafluoropropene (48.5 g, 0.32 mole) was added to the reactor over a 30 minute period and the reactor contents were held at 30° C. an additional 40 minutes. The reactor was cooled and the contents filtered into a 1-L separatory funnel and water washed four times, dried with anhydrous sodium sulfate and filtered. The material was shaken with anhydrous HF, water washed, dried with anhydrous sodium sulfate and filtered to give 125.6 g of C3F7OCHFCF2OC2H4OCF2CFHCF3 (86.3% pure). The material was fractionated in the concentric tube unit to give 72.3 g of C3F7OCHFCF2OC2H4OCF2CFHCF3 (95.3% purity) boiling at 194° C. Structure was confirmed by gc-ms. The viscosity was 48 centistokes (48×10−6 m2/s) at −50° C. measured using a Cannon-Fenske viscometer and a Wescan Model 221 viscosity timer.

Quelle