関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,5-Dimethoxyphenol | HCID 10383 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-6-fluorophenylacetic acid | HCID 123464 | — |
| 触媒 | Copper | HCID 23978 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(3,5-Dimethoxyphenoxy)-6-fluorophenyl acetic acid | HCID 54369342 | 86.1% |
反応手順
N,N-Dimethylformamide (20 ml) was added to 2-chloro-6-fluorophenyl acetic acid (3.77 g), 3,5-dimethoxyphenol (3.08 g), potassium carbonate (5.52 g), copper iodide (950 mg) and copper (250 mg), for stirring at 120° C. for 20 hours. The resulting reaction solution was partitioned with ethyl acetate and dilute hydrochloric acid, and the organic phase was washed in water and in a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate, to distill off the solvents under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=7:3), to recover 2-(3,5-dimethoxyphenoxy)-6-fluorophenyl acetic acid (5.27 g; yield of 86%). By 1H-NMR (90 MHz, CDCl3), the compound has the peaks shown below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05734067 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-83441b5019214471922280f5515c2e22 |
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| 出典メモ | uspto-grants-1998_03 |
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