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

HRID 1276569

반응식

HRID 1276569 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

Into a 1.3-liter stainless steel 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, 50° C. for 2 hr and 80° C. for 4 hr. The product was unloaded from the shaker tube and poured into ice water. The bottom organic layer was separated, washed with water and distilled to afford the title product (120 g, 40% yield) as a clear liquid, bp. 47° C./6.7 kPa. 19F NMR (188.24 MHz, CDCl3): -74.5 (m, 3F), -77.0 (m, AB-pattern, 2F), -148.2 (m, 1F), +49.7 (m, 1F).

후처리

  1. additionInto a 1.3-liter stainless steel tube was charged
  2. customThe tube was sealed
  3. temperaturecooled
  4. customThe bottom organic layer was separated
  5. washwashed with water
  6. distillationdistilled

출처 및 근거

ORD 기록
ord-13d3a2bcbb4b4bf4900d4d47989ac5e8
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166157

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