関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | 4-Fluorophenol | HCID 9732 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Nitrothiophene-2-carbonitrile | HCID 519294 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-(4-Fluorophenoxy)thiophene-2-carbonitrile | HCID 23130562 | 85.9% |
反応手順
To a dimethyl sulfoxide (100 mL) solution of 5-nitro-2-thiophene carbonitrile (5.00 g, 32.4 mmol) were added 4-fluorophenol (5.45 g, 48.6 mmol) and potassium carbonate (11.2 g, 81.0 mmol) under nitrogen atmosphere, which was stirred for 16 hours at 60° C. The reaction solution was cooled to room temperature and water was added, followed by extraction with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:10→1:5) to obtain the title compound (6.10 g, 85.9%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07691882B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-6a99905788ad4140bd2ffd2f0a2ea9e8 |
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| 出典メモ | uspto-grants-2010_04 |
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