関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Bromo-2-phenylpropanoic acid | HCID 228236 | — |
| 反応物 | 1,3-Dimethyl-6-(piperazin-1-yl)pyrimidine-2,4(1H,3H)-dione | HCID 12816873 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1,3-dimethyl-6-[4-(2-ethoxycarbonyl-2-phenylethyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione | HCID 19027085 | — |
反応手順
8.1 g of α-phenyl-β-bromopropionic acid and 1,3-dimethyl-6-(1-piperazinyl)-2,4(1H,3H)-pyrimidinedione were dissolved in 90 ml of dioxane, and the solution was stirred at 90° C. for 30 minutes. 12 ml of triethylamine was added to this solution, followed by stirring at 90° C. for 1 hour. Afterward, 60 ml of ethanol was added, and the solution was then heated under reflux for 3 hours. The solvent was distilled off from the reaction solution under reduced pressure, and the resulting residue was then dissolved in chloroform. The obtained solution was washed with water and then dried over anhydrous sodium sulfate. Afterward, the solvent was distilled off under reduced pressure, and the resulting residue was then purified through a silica gel column chromatograph (chloroform), thereby obtaining 4.5 g of 1,3-dimethyl-6-[4-(2-ethoxycarbonyl-2-phenylethyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05308848 |
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| 出典データセット | uspto-grants-1994_05 |
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| ORD ID | ord-b6179569103d4f128f1949b3660d7bb2 |
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| 出典メモ | uspto-grants-1994_05 |
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