Potassium Carbonate → CF3Cfhcf2CH2ocf2cfhocf3

HRID 638682

Reaction equation

HRID 638682 reaction equation
FC(F)(C)C(F)(F)C(F)(F)O.[C:12]([CH:16]([C:18]([CH2:21][OH:22])([F:20])[F:19])[F:17])([F:15])([F:14])[F:13].C(=O)([O-])[O-].[K+].[K+].[C:29]([O:33][C:34](=[C:36]([F:38])[F:37])[F:35])([F:32])([F:31])[F:30]>C(#N)C>[C:12]([CH:16]([C:18]([CH2:21][O:22][C:36]([CH:34]([O:33][C:29]([F:32])([F:31])[F:30])[F:35])([F:38])[F:37])([F:20])[F:19])[F:17])([F:15])([F:14])[F:13]

Participants

6

Reactant 4

HCID 11430Potassium CarbonateHCID 14474Perfluoro(methyl vinyl ether)HCID 5339902,2,3,4,4,4-Hexafluorobutan-1-olHCID 216527211,1,2,2,3,3-Hexafluorobutan-1-ol

Product 1

HCID 131728025CF3Cfhcf2CH2ocf2cfhocf3

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Conditions

Temperature
45 °C

Procedure

Hexafluorobutanol, CF3CFHCF2CH2OH (65.3 g, 0.34 mol), prepared essentially as described in Example 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.

Workup

  1. customThe resulting reaction mixture
  2. temperatureThe reactor was cooled
  3. filtrationthe contents of the reactor filtered
  4. customto remove the potassium carbonate
  5. additionThe resulting product-containing filtrate
  6. distillationwas distilled

Sources & evidence

ORD record
ord-1c1bafd3df174d5992769608d611e75f
Source dataset
uspto-grants-2010_04
Patent number
US07691282B2

Linked notes

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