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Hexafluoropropylene → 1,1,2,3,3,3-Hexafluoro-2-iodopropyl sulfurofluoridate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexafluoropropylene | HCID 8302 | — |
| 反応物 | Fluorosulfuric acid | HCID 24603 | — |
| 反応物 | Iodine chloride | HCID 24640 | — |
| 生成物 | 1,1,2,3,3,3-Hexafluoro-2-iodopropyl sulfurofluoridate | HCID 12596366 | 40% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06166157 |
| 出典データセット | uspto-grants-2000_12 |
| ORD ID | ord-13d3a2bcbb4b4bf4900d4d47989ac5e8 |
| 出典メモ | uspto-grants-2000_12 |