関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Cyanopyridine | HCID 7506 | — |
| 反応物 | 4-Aminobenzoic acid hydrazide | HCID 21450 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-[5-(Pyridin-4-yl)-1H-1,2,4-triazol-3-yl]aniline | HCID 20285812 | 20.9% |
反応手順
To 4-cyanopyridine (4.2 g.) in methanol (60 ml.) is added sodium (0.2 g.). The solution is allowed to stand for 0.5 hour at room temperature and is then added to a suspension of p-aminobenzhydrazide (6.4 g.) in 150 ml. of methanol. The resulting solution is heated 20 hours at reflux during which time a solid separates. The solid is filtered and heated to 245° C. over one hour and maintained at that temperature for an additional 15 minutes. After cooling the solid is recrystallized from a mixture of acetonitrile and water to yield 3-(p-aminophenyl)-5-(4-pyridyl)-1,2,4-triazole (2 g.) m.p. 251°-252.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04156085 |
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| 出典データセット | uspto-grants-1979_05 |
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| ORD ID | ord-6c938f77cc734dd4b30a2cac1a594e71 |
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| 出典メモ | uspto-grants-1979_05 |
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