関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Isopropyl isocyanate | HCID 61277 | — |
| 反応物 | HCID 178507748 | HCID 178507748 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178457923 | HCID 178457923 | 20% |
反応手順
A mixture containing 4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (0.2 g, 0.56 mmol) and isopropylisocyanate (0.155 g, 1.8 mmol) in 3 ml of dimethylformamide is heated at 100° C. for two hours then stirred at ambient temperature for two hours. 20 ml of water and 30 ml of ethyl acetate are added, followed by extraction, then the organic phase is washed with a saturated sodium chloride solution. The organic phase is dried over sodium sulfate. After evaporation to dryness, the oil obtained is triturated in isopentane. After filtration then drying, the solid obtained is purified on a silica column (eluent dichloromethane-ethanol-ammonia 96/2/2) and a pink-cream coloured powder is obtained with a yield of 20%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08188133B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-82406d6e907e43dfa1a27ad477627afd |
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| 出典メモ | uspto-grants-2012_05 |
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