参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 六甲基二硅氮烷 | HCID 13838 | — |
| 反应物 | C10-16-烷硫酸酯铵盐 | HCID 6097028 | — |
| 反应物 | 2-Acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester | HCID 69290800 | — |
| 产物 | Ethyl 1-cyclopropyl-2,5-dimethyl-1H-imidazole-4-carboxylate | HCID 45097089 | — |
反应步骤
Fine powdered ammonium sulfate (0.13 g, 1 mmol) was added to a suspension of Z)-2-acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester (7.0 g, 20 mmol) and hexamethyldisilazane (50 ml, 235 mmol) and refluxed over night at 145° C. The reaction mixture was evaporated and extracted with ethyl acetate and water. The organic phase was dried over sodium sulfate and evaporated. The crude product was purified by column chromatography on silica gel (ethyl acetate/methanol 4:1) and the desired compound was obtained as a light brown solid (1.3 g, 31%), MS: m/e=209.1 (M+H+).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US07091222B2 |
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| 来源数据集 | uspto-grants-2006_08 |
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| ORD ID | ord-ac2fb617a7cc49e7926340e6ef4fdd34 |
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| 来源说明 | uspto-grants-2006_08 |
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