関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N,N-Dimethylglycine | HCID 673 | — |
| 反応物 | 4-Bromobiphenyl | HCID 7101 | — |
| 反応物 | 4-Methoxyphenol | HCID 9015 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(4-Methoxyphenoxy)biphenyl | HCID 266864 | 132.3% |
反応手順
To a solution of 4-methoxyphenol (3.99 g, 32.17 mmol) and 4-bromobiphenyl (5 g, 21.45 mmol) in anhydrous dioxane (40 mL) were added cesium carbonate (13.98 g, 42.9 mmol) and N,N-dimethylglycine.HCl (0.898 g, 6.4 mmol). The reaction mixture was flushed with nitrogen. Copper (I) iodide (0.408 g, 2.145 mmol) was added and the reaction mixture was stirred at 90° C. for 18 h under an atmosphere of nitrogen. The mixture was diluted with water (100 mL) and extracted with EtOAc (250 mL). Aqueous layer was re-extracted with EtOAc (150 mls). The organic layers were combined, dried over anhydrous Na2SO4, and concentrated to obtain the title product 7.84 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07402684B2 |
|---|
| 出典データセット | uspto-grants-2008_07 |
|---|
| ORD ID | ord-911a70802ff449069dc709acb0634781 |
|---|
| 出典メモ | uspto-grants-2008_07 |
|---|
