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

HRID 963581

反応式

HRID 963581 の反応式
[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]

参加物

4

反応物 3

HCID 8302HexafluoropropyleneHCID 24603Fluorosulfuric acidHCID 24640Iodine chloride

生成物 1

HCID 125963661,1,2,3,3,3-Hexafluoro-2-iodopropyl sulfurofluoridate収率 40%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6e932b3e40b94f14a27d3f27a04e332e
出典データセット
uspto-grants-1998_06
特許番号
US05763552

関連ノート

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