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

HRID 963581

반응식

HRID 963581 반응식
[I:1]Cl.[F:3][S:4]([OH:7])(=[O:6])=[O:5].[F:8][C:9]([F:16])([F:15])[C:10]([F:14])=[C:11]([F:13])[F:12]>>[S:4]([F:3])([O:7][C:11]([F:13])([F:12])[C:10]([F:14])([I:1])[C:9]([F:16])([F:15])[F:8])(=[O:6])=[O:5]

참가 물질

4

반응물 3

HCID 8302HexafluoropropyleneHCID 24603Fluorosulfuric acidHCID 24640Iodine chloride

생성물 1

HCID 125963661,1,2,3,3,3-Hexafluoro-2-iodopropyl sulfurofluoridate수율 40%

실험 절차

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.

후처리

  1. additionA 1.3-liter stainless steel shaker tube was charged
  2. customThe tube was sealed
  3. temperaturecooled
  4. waitat 80° C. for 4 hr
  5. washwashed with water
  6. distillationdistilled

출처 및 근거

ORD 기록
ord-6e932b3e40b94f14a27d3f27a04e332e
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763552

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