Hexafluoropropylene → 1,1,2,3,3,3-Hexafluoro-2-iodopropyl sulfurofluoridate

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Reaction Steps

A 1.3-liter stainless steel shaker tube was charged a mixture of iodine monochloride (130 g, 0.80 mol) and fluorosulfonic acid (88 g, 0.88 mol). The tube was sealed and cooled, then hexafluoropropylene (144 g, 0.96 mol) was transferred into the tube. The reaction mixture was kept at 25° C. for 2 hr, at 50° C. for 2 hr, and at 80° C. for 4 hr. The product unloaded from the shaker tube was poured into ice water, and the bottom organic layer was separted, washed with water, and distilled to give 120 g of 2-iodo-hexafluoropropyl fluorosulfate (formula above, 40% yield) as a clear liquid having a boiling point of 47° C. at 50 mmHg.

Provenance & Evidence