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Hydrazine hydrate (1:1) → N-[1-(5-Oxo-3-phenyl-4,5-dihydro-1,2,4-triazin-6-yl)propyl]cyclopentanecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Benzamidine, hydrochloride | HCID 80289 | — |
| 反応物 | Ethyl 3-[(cyclopentylcarbonyl)amino]-2-oxopentanoate | HCID 21991319 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-[1-(5-Oxo-3-phenyl-4,5-dihydro-1,2,4-triazin-6-yl)propyl]cyclopentanecarboxamide | HCID 135752529 | — |
反応手順
3.5 g (22.3 mmol, 1 equiv.) benzenecarboximidamide hydrochloride are suspended in 10 ml of ethanol and 1.37 g (26.8 mmol, 1.2 equiv.) hydrazine hydrate are added. After stirring at room temperature for 1 hour, 6.28 g (24.6 mmol, 1.1 equiv) of ethyl 3-[(cyclopentylcarbonyl)amino]-2-oxopentanoate (Example 99A), dissolved in 40 ml of ethanol, are added. The reaction mixture is stirred at 70° C. (bath temperature) for 4 hours. The mixture is evaporated to dryness in vacuo and the product is purified by chromatography (flash or column chromatography or preparative HPLC).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087605B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-ac4239c9e35d4f9abbabb31f98870e4d |
| 出典メモ | uspto-grants-2006_08 |