化工社化工社 化学情報印刷レポート · 研究参考用
Cesium carbonate → 1-Bromo-4-(2,4-difluorophenoxy)-2-fluoro-5-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2,4-Difluorophenol | HCID 123051 | — |
| 反応物 | 1-Bromo-2,4-difluoro-5-nitrobenzene | HCID 223078 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-Bromo-4-(2,4-difluorophenoxy)-2-fluoro-5-nitrobenzene | HCID 90415995 | — |
| 生成物 | 1-Bromo-2-(2,4-difluorophenoxy)-4-fluoro-5-nitrobenzene | HCID 90418619 | — |
反応手順
A mixture of 1-bromo-2,4-difluoro-5-nitrobenzene (0.5 g, 2.10 mmol) and cesium carbonate (0.685 g, 2.10 mmol) in DMSO (10.50 mL) was treated dropwise with 2,4-difluorophenol (0.273 g, 2.10 mmol), stirred for 60 minutes at ambient temperature and partitioned between ethyl acetate and water, adjusting the pH to 6 with 1 M HCl. The organic layer was washed with water, saturated aqueous sodium chloride, dried (MgSO4), filtered, and concentrated. Purification by chromatography (silica gel, 0-30% ethyl acetate in heptanes) afforded the title compound and 1-bromo-4-(2,4-difluorophenoxy)-2-fluoro-5-nitrobenzene as an inseparable mixture (0.59 g, 81%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09321764B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-5e93caf2891d47e6b8f113ebe17841b7 |
| 出典メモ | uspto-grants-2016_04 |