関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-6-(2-Thienylmethoxy)Pyridine | HCID 18186944 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(2-Thienylmethyloxy)-6-(meta-trifluoromethylphenoxy)pyridine | HCID 19957396 | — |
反応手順
To a solution containing meta-trifluoromethylphenol (3.62 g, 0.0045×5.0 mol), sodium hydride (0.36 g, (Ca.60% in mineral oil), 0.0045×2.0 mol) and CuI (0.42 g, 0.0045×0.5 mol) in dimethylformamide, 2-chloro-6-(2-thienylmethyloxy)pyridine (1.0 g, 0.0045 mol) was added and the resultant solution was refluxed for about 3 hours. Additional sodium hydride (0.36 g, (60% in mineral oil), 0.0045×2.0 mol) was added thereto and the resultant solution was refluxed for another about 1 hour, thereafter the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The obtained organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and thereafter, concentrated and purified on a silica gel column to obtain the end product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05624942 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-cb0f05a242d24a13a620fc4ecb1f7367 |
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| 出典メモ | uspto-grants-1997_04 |
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