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

HRID 1276569

反応式

HRID 1276569 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

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).

後処理

  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

出典と根拠

ORDレコード
ord-13d3a2bcbb4b4bf4900d4d47989ac5e8
出典データセット
uspto-grants-2000_12
特許番号
US06166157

関連ノート

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