Carbon Dioxide → HCID 22987397, compound

HRID 1937266Notes

Reaction equation

HRID 1937266 reaction equation
[F-:1].[K+].C(=O)=O.[C:6]([O:10][C:11]([C:14]([C:17](F)=[O:18])([F:16])[F:15])([F:13])[F:12])([F:9])([F:8])[F:7].[F:20][C:21]([F:28])([F:27])[C:22]([F:26])=[C:23]([F:25])[F:24]>COCCOCCOC>[F:13][C:11]([F:12])([O:10][C:6]([F:7])([F:8])[F:9])[C:14]([F:15])([F:16])[C:17](=[O:18])[C:22]([F:26])([C:23]([F:1])([F:25])[F:24])[C:21]([F:28])([F:27])[F:20]

Participants

6

Reactant 4

HCID 280Carbon DioxideHCID 8302HexafluoropropyleneHCID 120237Perfluoromethoxypropionyl fluorideHCID 522689Potassium Fluoride

Product 1

HCID 22987397HCID 22987397, compoundYield 130.9%

Reagents, catalysts & solvents 1

HCID 8150DiglymeSolvent

Procedure

Into a clean dry 600 mL Parr reactor were added 11.6 g (0.20 mol) of anhydrous potassium fluoride and 113.5 g of anhydrous diglyme. The contents of the reactor were stirred and cooled with dry ice, then 230 g (0.96 mol) of CF3OCF2CF2COF (available from 3M Co., approximately 97 percent purity) was added to the sealed reactor using isolated vacuum. With the reactor at 80° C. and pressure of 80 psig (4900 torr), 154 g (1.03 mol) of hexafluoropropylene was gradually added over a 3½ hour period. Following a one hour reaction hold time, the product was recovered from the reaction mixture by distillation and phase split prior to fractionation to give 100 g of 1,1,2,2,4,5,5,5-octafluoro-1-trifluoromethoxy-4-trifluoromethylpentan-3-one, having a boiling point of 77° C. and a purity of 99.8% as determined by gas chromatography. The structure was confirmed by gas chromatography and mass spectroscopy.

Workup

  1. customInto a clean dry 600 mL Parr reactor
  2. customusing isolated vacuum
  3. customreaction hold time
  4. distillationthe product was recovered from the reaction mixture by distillation and phase
  5. customsplit

Sources & evidence

ORD record
ord-b520b0aac0294a75a8f64ffde470ad37
Source dataset
uspto-grants-2002_05
Patent number
US06394107B1

Reaction notes

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