化工社化工社 化学情報印刷レポート · 研究参考用
4-Bromo-2-fluorophenol → 4-Bromo-2-fluoro-1-(5,5,6,6,7,7,8,8,8-nonafluoro-octyloxy)-benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Bromo-2-fluorophenol | HCID 2724981 | — |
| 反応物 | 4-(5,5,6,6,7,7,8,8,8-Nonafluoro-octyloxy)-tosylate | HCID 86759366 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Cesium carbonate | HCID 10796 | — |
| 生成物 | 4-Bromo-2-fluoro-1-(5,5,6,6,7,7,8,8,8-nonafluoro-octyloxy)-benzene | HCID 20632168 | — |
反応手順
To a solution of commercially available 4-bromo-2-fluorophenol (25) (1 equi.) and 4-(5,5,6,6,7,7,8,8,8-nonafluoro-octyloxy)-tosylate (10) (1 equi.) in DMF (3 mL/mmole), cesium carbonate (1.25 equi.) was added at room temperature. The reaction mixture was stirred at that temperature for 24 h, quenched with water, extracted with ethyl acetate:hexane(1:1), washed with brine, dried over MgSO4, and concentrated in vacuo. Purification by chromatography on silica gel (5% EtOAc/hexanes) and recrystallization from acetonitrile afforded 4-bromo-2-fluoro-1-(5,5,6,6,7,7,8,8,8-nonafluoro-octyloxy)-benzene (26) a colorless oil (87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06703082B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-7621395f5351427bb19466a439f4e866 |
| 出典メモ | uspto-grants-2004_03 |