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HRID 447803作成日:2026年10月25日
Water → 5-Chloro-1-(5-chloro-2-(methylsulfonyl)benzyl)-2-imino-1,2-dihydropyridine-3-carboxamide hydrochloride
https://huagongshe.com/reaction/447803
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Cyano-2-(3,4-dichloro-5(2H)-oxo-2-furyl)acetamide | HCID 541792 | — |
| 反応物 | 1-[5-Chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride | HCID 66969896 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-Chloro-1-(5-chloro-2-(methylsulfonyl)benzyl)-2-imino-1,2-dihydropyridine-3-carboxamide hydrochloride | HCID 66970086 | 89.9% |
反応手順
(Step 4) To a suspension of 2-cyano-2-(3,4-dichloro-5-oxo-2,5-dihydrofuran-2-yl)acetamide (0.28 g) and 1-[5-chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride obtained in Step 3 (0.26 g) in ethanol (3 ml) was added N,N-diisopropylethylamine (0.44 ml) at room temperature, and the resulting mixture was heated under reflux for 4 hr. The reaction mixture was treated with water and stirred at 70° C. for 1 hr. After cooling to room temperature, the precipitate was collected by filtration and dried. The precipitate was suspended in methanol, and treated with a 2 M hydrogen chloride-methanol solution (0.3 ml). The resulting mixture was stirred at room temperature overnight. The precipitate was collected by filtration and dried to give the title compound (0.22 g) as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481569B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-56ed163206734d0fbcd7db865f382310 |
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| 出典メモ | uspto-grants-2013_07 |
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