関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | Cyclooctanone | HCID 10403 | — |
| 反応物 | Ammonium Carbonate | HCID 517111 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,3-Diazaspiro(4.7)dodecane-2,4-dione | HCID 95195 | 73% |
反応手順
To a mixture of cyclooctanone (RA 17 g, 135 mmol, Sigma-Aldrich) in ethanol (200 mL) and water (200 mL) were added KCN (17.5 g, 269 mmol, Sigma-Aldrich) followed by ammonium carbonate ([NH4]2CO3, 51.8 g, 539 mmol, Sigma-Aldrich). The resulting reaction mixture was stirred at 80° C. for 6 h. The reaction mixture was evaporated to dryness under reduced pressure to provide a white solid precipitate which was filtered, collected, and dried for 16 h to provide 15.9 g of the compound of formula RB, 1,3-diazaspiro[4.7]dodecane-2,4-dione (yield 73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08637502B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-c6ac9c4851a143f98c389a055d7e72a3 |
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| 出典メモ | uspto-grants-2014_01 |
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