関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Acetohydrazide | HCID 14039 | — |
| 反応物 | 4-(pentylamino)-1H-imidazole-5-carbonitrile | HCID 45120565 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178446281 | HCID 178446281 | 10% |
反応手順
To the mixture of 4-(pentylamino)-1H-imidazole-5-carbonitrile (0.40 g, 2 mmol), acetic acid, hydrazide (0.33 g, 4.5 mmol) in1-butanol (10 mL) was added potassium carbonate (0.10 g, 0.72 mmol). The mixture was sealed and stirred at 165° C. for 14 hours. The reaction mixture was diluted with water and extracted with ethyl acetate three times. The combined organic layers were dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by preparative LCMS (method A) to yield the desired product (45 mg, 10% yield). LCMS calculated for C11H19N6(M+H): 235.2. found: 235.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07863285B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-95788f4ba37f4631910b700d19ca189b |
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| 出典メモ | uspto-grants-2011_01 |
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