ChemicalBook CAS DataBase List 5-IODOOCTAFLUORO-3-OXAPENTANESULFONYL FLUORIDE

5-IODOOCTAFLUORO-3-OXAPENTANESULFONYL FLUORIDE synthesis

3synthesis methods

Product Name:5-IODOOCTAFLUORO-3-OXAPENTANESULFONYL FLUORIDE
CAS Number:66137-74-4
Molecular formula:C4F9IO3S
Molecular Weight:426

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5-IODOOCTAFLUORO-3-OXAPENTANESULFONYL FLUORIDE

66137-74-4
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$25.00/1 g

Yield: 56%

Reaction Conditions:

Stage #1:tetrafluoroethane-β-sultone with potassium fluoride in diethylene glycol dimethyl ether at 20; for 0.5 h;Autoclave;Cooling with ice;
Stage #2: with bromine;iodine in diethylene glycol dimethyl ether at 20; under 3000.3 Torr; for 24 h;Cooling with ice;Inert atmosphere;

Steps:

2 Example 2
In a 300 mL autoclave equipped with a pressure gauge and a stirrer, 7.2 g (120 mmol, 1.0 eq.) Of potassium fluoride,And 40 g of diglyme were added. Next, under ice bath cooling,With stirring, 22 g (120 mmol, 1.0 eq.) Of tetrafluoroethane β-saltone was added dropwise over 3 minutes,It was returned to room temperature over 30 minutes. 38 g (150 mmol, 1.2 eq.) Of iodine, 5.0 g (31 mmol, 0.25 eq.) Of bromine and 40 g of diglyme were added, and the mixture was cooled with an ice bath.The gas phase was replaced with nitrogen. The gas phase part was evacuated (-0.08 MPaG) and returned to room temperature, and then TFE was pressure-fitted to 0.40 MPaG. The operation of press-fitting TFE to 0.40 MPaG every hour at room temperature for 12 hours was repeated.After further stirring for 12 hours at room temperature, the reaction was stopped by replacing the gas phase with nitrogen.The reaction solution was added dropwise to a container containing water (100 g) and chloroform (100 g), and the lower layer was washed with a 1M potassium sulfite aqueous solution (100 g) and water (100 g).It was dried over magnesium sulfate.The solvent was distilled off under reduced pressure, and 30 g of a compound represented by FSO2CF2CF2OCF2CF2I having a purity of 98% was obtained by vacuum distillation.(Yield 56%).

References:

Daikin Industries Ltd;Asahi Kasei Corporation;Kishimoto, Masayuki;Tomita, Masahiro;Nakagami, Tsubasa;Nagato, Yasuhiro JP2020/50600, 2020, A Location in patent:Paragraph 0041