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Methyl 4-fluorobenzoylacetate → 1-(5-Chloro-2,4-dimethoxy-phenyl)-5-(4-fluoro-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 4-fluorobenzoylacetate | HCID 579425 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | 1-Azido-5-chloro-2,4-dimethoxybenzene | HCID 58731017 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(5-Chloro-2,4-dimethoxy-phenyl)-5-(4-fluoro-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid | HCID 58731018 | — |
反応手順
1-Azido-5-chloro-2,4-dimethoxy-benzene (0.4 g, 1.9 mmol), 3-(4-Fluoro-phenyl)-3-oxo-propionic acid methyl ester (0.42 g, 2.2 mmol) and sodium ethoxide in EtOH (70 mg of sodium in 15 mL EtOH) were refluxed for 3 hours. During the reaction, the solution turned brown from dark green. After that, EtOH was evaporated off and the resulting oil was dried in vacuum. Trituration with ether (15 mL) gave light brown solids, which were removed by filtration and washed with ether. The solids then re-dissolved in CHCl3 and filtered. After evaporation of the solvent, light brown solids were obtained (0.35 g, 50%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728016B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-7a8b9422f4634db6947a7b29d86ba228 |
| 出典メモ | uspto-grants-2010_06 |