化工社化工社 化学情報印刷レポート · 研究参考用
Cesium carbonate → 5-(5,5,6,6,7,7,8,8,8-Nonafluoro-octyloxy)-2-(4-oct-7-enyloxy-phenyl)-pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 8-Bromooct-1-ene | HCID 75907 | — |
| 反応物 | 4-[5-(5,5,6,6,7,7,8,8,8-Nonafluorooctyloxy)-pyrimidin-2-yl]-phenol | HCID 135585897 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 5-(5,5,6,6,7,7,8,8,8-Nonafluoro-octyloxy)-2-(4-oct-7-enyloxy-phenyl)-pyrimidine | HCID 23509148 | — |
反応手順
A suspension of 8-bromo-1-octene (1.00 g, 5.24 mmol), 4-[5-(5,5,6,6,7,7,8,8,8-nonafluorooctyloxy)-pyrimidin-2-yl]-phenol (2.54 g, 5.50 mmol) and cesium carbonate (3.40 g, 10.47 mmol) in acetone (40 ml) was heated under reflux for 12 h, cooled to room temperature, washed with water and the organic layer extracted into ethyl acetate/hexane (3 times). The combined organic extracts were washed with brine, dried (MgSO4) and the solvent removed in vacuo. The residues were purified by column chromatography [silica gel, eluted with hexane/ethyl acetate (9:1)] to yield a colorless solid, which was recrystallized from ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06759101B2 |
| 出典データセット | uspto-grants-2004_07 |
| ORD ID | ord-6135afe76c5649b3a09bdfc2fe24d82a |
| 出典メモ | uspto-grants-2004_07 |