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Tetrahydrofuran → Potassium 1,1,2,2-tetrafluoro-2-(pentafluoroethoxy)ethane-1-sulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 1,1,2,2-tetrafluoro-2-(1,1,2,2,2-pentafluoroethoxy)ethanesulfonyl Fluoride | HCID 2782567 | — |
| 反応物 | Potassium trimethylsilanolate | HCID 23668039 | — |
| 溶媒 | Glycerol | HCID 753 | — |
| 生成物 | Potassium 1,1,2,2-tetrafluoro-2-(pentafluoroethoxy)ethane-1-sulfonate | HCID 2782415 | 65% |
反応手順
The procedure of Example 1 was followed using perfluoro-3-oxapentanesulfonyl fluoride (7.95 g, 25 mmol), potassium trimethylsilanolate (3.2 g, 25 mmol) and dry tetrahydrofuran (100 mL) while heating at reflux for 1.5 h. Potassium perfluoro-3-oxapentanesulfonate (3.79 g initially and 1.74 g by concentrating the filtrate under vacuum; total 5.53 g, 65% yield) was isolated as a white solid: 19F NMR (fluorotrichloromethane) δ -79.4 (m, CF2, 2F), -83.2 (s, CF3, 3F), -84.9 (m, CF2, 2F), -115.0 ppm (m, CF2, 2F); Positive ion Fast Atom Bombardment MS (Glycerol matrix, Cs⊕ ion bombardment) m/e 393, 747, 1101, 1455, 1809 for M+K⊕ to M5 +K⊕.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04723016 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-bced94d3b141486e89edeb33840b194b |
| 出典メモ | uspto-grants-1988_02 |