関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzoylhydrazine | HCID 11955 | — |
| 反応物 | 4-(pentylamino)-1H-imidazole-5-carbonitrile | HCID 45120565 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-pentyl-5-(3-phenyl-1H-1,2,4-triazol-5-yl)-1H-imidazol-4-amine | HCID 135984693 | 17% |
反応手順
The mixture of 4-(pentylamino)-1H-imidazole-5-carbonitrile (200 mg, 1.12 mmol), benzohydrazide (229 mg, 1.68 mmol) and potassium carbonate (100 mg, 0.72 mmol) in 1-butanol (6 ml) in a sealed tube was stirred at 170° C. for 14 hours. The reaction was diluted with water and extracted with EtOAc three times. The combined organic layers was dried with sodium sulfate, filtered, and concentrated in vacuo. The crude residue was purified by preparative LCMS (method A) to yield the desired product (50 mg, 17% yield). LCMS calculated for C16H21N6 (M+H): 297.2. found 297.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07902205B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-de2fef636ebd4dc388da89a844b71e8d |
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| 出典メモ | uspto-grants-2011_03 |
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