Reaction #1797480

Reaction equation

potassium carbonate

CF3OCF═CF2

Hexafluorobutanol

CF3CFHCF2CH2OH

→

CF3CFHCF2CH2OCF2CFHOCF3

Solvents

acetonitrile

Conditions

Workup

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

Procedure

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.

Source