関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Cyanide | HCID 768 | — |
| 反応物 | Isophorone | HCID 6544 | — |
| 反応物 | 1,3-Dimethylimidazolium-4-carboxylate | HCID 479951 | — |
| 生成物 | 3-Cyano-3,5,5-trimethylcyclohexanone | HCID 99068 | — |
反応手順
622 g (4.5 mol) of isophorone and 3.61 g (25.8 mmol) of 1,3-dimethylimidazolium-4-carboxylate were placed in a reaction vessel and a mixture of 207.3 g (1.5 mol) of isophorone and 81.0 g (3 mol) of hydrogen cyanide was added at 120° C. over a period of about 60 minutes. The mixture was subsequently stirred further for about 60 minutes at 120° C. After cooling, the HCN concentration was determined by titration. Free hydrocyanic acid could no longer be detected (HCN conversion>99.9%). After addition of 2.0 g of 85% strength H3PO4, the reaction product was distilled at 0.1 hPa. This gave 484 g of 3-cyano-3,5,5-trimethylcyclohexanone (97.7% based on HCN used).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06022988 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-5458b9ee312d4a08b25f9924346ae0fb |
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| 出典メモ | uspto-grants-2000_02 |
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