Difluoro(fluorosulphonyl)acetyl fluoride → HCID 21940881, compound

HRID 2216230Notes

Reaction equation

HRID 2216230 reaction equation
[C:1]([O-:4])([O-:3])=O.[C:5]([O-:8])([O-])=[O:6].OO.OO.OO.[Na+].[Na+].[Na+].[Na+].[F:19][S:20]([C:23](C(F)=O)([F:25])[F:24])(=[O:22])=[O:21]>C(Cl)(F)(F)C(Cl)(Cl)F>[F:25][C:23]([F:24])([S:20]([F:19])(=[O:21])=[O:22])[C:1]([O:4][O:8][C:5](=[O:6])[C:23]([F:25])([F:24])[S:20]([F:19])(=[O:22])=[O:21])=[O:3]

Participants

4

Reactant 2

HCID 69614Difluoro(fluorosulphonyl)acetyl fluorideHCID 159762Sodium percarbonate

Product 1

HCID 21940881HCID 21940881, compoundYield 42%

Reagents, catalysts & solvents 1

HCID 6428Cfc 113Solvent

Conditions

Temperature
0 °C

Procedure

A round-bottom flask is charged with 50 ml of CFC-113 and 2.0 g of sodium percarbonate (13 mmoles or 19 mmoles of H2O2 equivalent). After chilling the contents of the flask to 0° C., 2.83 ml of FSO2CF2(C═O)F (25 mmoles) is added and the resulting slurry is stirred magnetically for 3 hours. The reaction mixture is filtered through a pad of Drierite® on glass wool, washing through with fresh CFC-113, an operation assumed to remove any unreacted percarbonate and any free H2O2. The filtrate, now measuring 52 ml in volume, is found to be 0.10 M in peroxide for a 42% yield based on starting FSO2CF2(C═O)F.

Workup

  1. filtrationThe reaction mixture is filtered through a pad of Drierite® on glass wool
  2. washwashing through with fresh CFC-113
  3. customto remove any unreacted percarbonate

Sources & evidence

ORD record
ord-5210efb40b7e4edcbb99630896323245
Source dataset
uspto-grants-2006_09
Patent number
US07112314B2

Reaction notes

Loading…