関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Bromo-1-propanol | HCID 12308 | — |
| 反応物 | 1,3-Dimethyl-6-(piperazin-1-yl)pyrimidine-2,4(1H,3H)-dione | HCID 12816873 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1,3-dimethyl-6-[4-(3-hydroxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione | HCID 10356417 | 69.9% |
反応手順
14.1 g of 1,3-dimethyl-6-(1-piperazinyl)-2,4(1H,3H)-pyrimidinedione (compound b), 11.7 g of 3-bromo-1-propanol and 13 g of triethylamine were heated under reflux in 250 ml of ethanol for 20 hours to carry out reaction. After completion of the reaction, the resultant reaction mixture was then concentrated to dryness, and the resultant residue was dissolved in 300 ml of chloroform and then washed with 100 ml of water twice. The washed organic layer was dried over anhydrous magnesium sulfate and then treated with under reduced pressure, and the solvent was distilled off, thereby obtaining 20.5 g of a crude product. Next, ether was added to this crude product so as to achieve crystallization. The resultant crystals were recovered, washed and then dried to obtain 12.4 g (yield 69.8%) of 1,3-dimethyl-6-[4-(3-hydroxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound a).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05332739 |
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| 出典データセット | uspto-grants-1994_07 |
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| ORD ID | ord-cf7899b4daba42128b0d0ce1d47c0936 |
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| 出典メモ | uspto-grants-1994_07 |
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