関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 5-[4-(2-Bromophenyl)-4h-1,2,4-triazol-3-yl]-2-phenylpyridine | HCID 22019260 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 5-[5-bromo-4-(2-bromophenyl)-4H-1,2,4-triazol-3-yl]-2-phenylpyridine | HCID 22019229 | 69% |
反応手順
5-[4-(2-Bromophenyl)-4H-1,2,4-triazol-3-yl]-2-phenylpyridine prepared in the Production Example 2 was dissolved in a mixture solvent of carbon tetrachloride (100 ml) and acetic acid (100 ml), followed by addition of n-bromosuccinimide (5.90 g), and refluxed under heating for 3 hours. After the reaction solution was cooled to ambient temperature, the solution was concentrated-under reduced pressure. Saturated aqueous sodium hydrogen carbonate solution was added to the resulting residue, and extracted with chloroform. Subsequently, the organic layer was dried over anhydrous magnesium sulfate. After the solvent was evaporated under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=3/1), to afford the entitled compound as yellow solid (6.96 g, 69%). The physico-chemical values are as follows.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084164B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-ffac4d3930b0426da52d569c2e6fa4ff |
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| 出典メモ | uspto-grants-2006_08 |
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