関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyrohydrazide | HCID 77079 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 1-(Pyrimidin-2-yl)piperidine-4-carboxylic acid | HCID 2767267 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 1-Pyrimidin-2-yl-piperidine-4-carboxylic acid N'-butyryl-hydrazide | HCID 23544069 | 62% |
反応手順
A mixture of 1-pyrimidin-2-yl-piperidine-4-carboxylic acid (3.0 g, 14.5 mmol)(see reference U.S. Pat. No. 4,826,843), 1-hydroxybenzotriazole hydrate (1.96 g, 14.5 mmol) and 1-(3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (2.78 g, 14.5 mmol) in dichloromethane (100 ml) was stirred for 10 minutes. Butyric acid hydrazide (1.78 g, 17.4 mmol) was added and the reaction mixture was stirred under a nitrogen atmosphere for 18 hours. The reaction mixture was diluted with dichloromethane (100 ml) and sodium hydrogen carbonate solution was added. The reaction mixture was concentrated under reduced pressure and the solid formed was isolated by filtration. The material obtained was dried under vacuum at 40° C. to give the title compound (2.62 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084145B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-4e299013dbfd48c1bf2a6e7afd13ee69 |
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| 出典メモ | uspto-grants-2006_08 |
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