関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Cyanopyridine | HCID 7506 | — |
| 反応物 | 2-Methylisonicotinic acid hydrazide | HCID 322549 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-methyl-4-(3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)pyridine | HCID 20309749 | — |
反応手順
Sodium (0.4 grams) is added to 4-cyanopyridine (8.3 grams, 0.08 mole) in methanol, and the solution is allowed to stand 30 minutes at room temperature. A suspension of 2-methylisonicotinic acid hydrazide (0.07 mole) in methanol (160 ml.) is added, and the resulting solution is heated at reflux for 30 minutes. After cooling, the intermediate acylamidrazone is collected by filtration. The acyclic intermediate is then heated at 260°C. for 15 minutes, after which the reaction is cooled to room temperature. Upon recrystallization from acetonitrile-water, 5-(4-pyridyl)-3-(2-methyl-4-pyridyl)-1,2,4-triazole is obtained, m.p. 245°-248°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03947577 |
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| 出典データセット | uspto-grants-1976_03 |
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| ORD ID | ord-73a8b91493344a939b95fabac04cf42b |
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| 出典メモ | uspto-grants-1976_03 |
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