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-Fluoroiodobenzene | HCID 9605 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Fluoro-6-methoxyphenol | HCID 2737367 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Fluoro-2-(4-fluoro-phenoxy)-3-Methoxy benzene | HCID 57701118 | 6,350.2% |
反応手順
To a suspension of 2-fluoro-6-methoxy phenol (1) (2.8 g, 20 mmol), N,N-dimethyl glycine.HCl (837 mg, 6 mmol), Cs2CO3 (13 g, 40 mmol), 1-fluoro-4-iodobenzene (2.3 mL, 20 mmol), in Dioxane (40 ml) was added copper iodone (381 mg, 2 mmol). The reaction mixture was stirred at 105° C. over 1 week. Upon heating the reaction mixture turned from brown to a bright green. After cooling to room temperature, the reaction mixture was filtered and the filtrate was concentrated in-vacuo. The crude was purified by silica gel eluted with hexane/EtOAc (10:1), concentrated in-vacuo, to provide 300 g (21% yield) of product (2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08877816B2 |
|---|
| 出典データセット | uspto-grants-2014_11 |
|---|
| ORD ID | ord-6114c9b5157c4a06afa58a4a0bff2316 |
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| 出典メモ | uspto-grants-2014_11 |
|---|
