関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 4'-Fluoro-3'-nitroacetophenone | HCID 2734612 | — |
| 反応物 | Ethyl 3-(1H-imidazol-2-YL)propanoate | HCID 22259341 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Ethyl 3-[1-(4-acetyl-2-nitrophenyl)-1H-imidazol-2-yl]-propanoate | HCID 59198914 | 69% |
反応手順
A mixture of 4′-fluoro-3′-nitroacetophenone 2.04 g, ethyl 3-(1H-imidazol-2-yl)propanoate 1.87 g, potassium carbonate 3.07 g and N,N-dimethylacetamide 28 mL was heated at 100° C. for 16.5 hours. The reaction liquid was allowed to cool off and to which 60 mL of diethyl ether was added, followed by filtration. Adding 100 mL of water to the filtrate, the organic layer was separated. The aqueous layer was extracted with 100 mL of diethyl ether. The extract was combined with the organic layer, washed twice with 20 mL of water and once with 10 mL of saturated brine by the order stated, and dried over magnesium sulfate. Distilling the solvent off under reduced pressure, 2.54 g of the title compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829000B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-26b8b4cf5263426fbdedf8d120e736dd |
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| 出典メモ | uspto-grants-2014_09 |
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