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HRID 573922作成日:2026年10月26日
1,2-Dibromopropane → (1Z)-1-[3-(2-ethyl-5-methylphenyl)-4-methyl-1,3-thiazolidin-2-ylidene]-3-[2-[4-[1-[4-(trifluoromethoxy)phenyl]-1,2,4-triazol-3-yl]phenyl]ethyl]urea
https://huagongshe.com/reaction/573922
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dibromopropane | HCID 6553 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-(4-(2-Isocyanatoethyl)phenyl)-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole | HCID 90404408 | — |
| 反応物 | 1-(2-Ethyl-5-methylphenyl)thiourea | HCID 90404560 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | (1Z)-1-[3-(2-ethyl-5-methylphenyl)-4-methyl-1,3-thiazolidin-2-ylidene]-3-[2-[4-[1-[4-(trifluoromethoxy)phenyl]-1,2,4-triazol-3-yl]phenyl]ethyl]urea | HCID 90412375 | 13.3% |
反応手順
3-(4-(2-Isocyanatoethyl)phenyl)-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole (C34a)(0.16 g, 0.42 mmol), 1-(2-ethyl-5-methylphenyl)thiourea (CA41) (0.081 g, 0.42 mmol), and cesium carbonate (0.13 g, 0.39 mmol) in acetonitrile (1.9 mL) was stirred at room temperature for 3 hours. The reaction was diluted with butanone (2 mL) and potassium carbonate (0.12 g, 0.83 mmol) and 1,2-dibromopropane (0.090 mL, 0.83 mmol) were added. The reaction was heated to 60° for 6 hours. The reaction was diluted with water and extracted with dichloromethane (2×) and the organic layers were filtered through a phase separator and concentrated. Purification by flash column chromatography using 0-100% ethyl acetate/B, where B=1:1 dichloromethane/hexanes, as eluent provided the title compound as a yellow oil (0.034 g, 13%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09029560B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-e4f714b057a64eeb980a51783f9a5f4c |
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| 出典メモ | uspto-grants-2015_05 |
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