関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 2-Oxocyclohexanepropiononitrile | HCID 96223 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 生成物 | Decahydroquinoline | HCID 92911 | 7.9% |
| 生成物 | 2-(3-Aminopropyl)-cyclohexylamine | HCID 10888155 | 86.3% |
反応手順
Through a tubular reactor (diameter 16 mm, packing height 50 cm, oil-heated double jacket), installed up-stream of the hydrogenation reactor and packed with 70.0 g (100 g) of γ-aluminum oxide in he form of 1.5 mm extrudates, there were passed upwardly, per hour, 10.7 g of 2-(2-cyanoethyl)-cyclohexanone (purity 97.5%, 0.069 mole) and 500 ml of liquid ammonia (300 g, 17.6 moles) at a pressure of 250 bar and a temperature of 80° C. Hydrogen was then added to the stream at a rate of 60 standard liters (2.7 moles) per hour, and the effluent from the in-line imination reactor was passed upwardly through the hydrogenation reactor at a pressure of 250 bar and a temperature of 130° C. Gas-chromatographic analysis of the hydrogenation product gave 86.3% of 2-(3-aminopropyl)-cyclohexylamine and 7.9% of decahydroquinoline, corresponding to a yield of 2-(3-aminopropyl)-cyclohexylamine of 87.1% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05239120 |
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| 出典データセット | uspto-grants-1993_08 |
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| ORD ID | ord-fae9fc7000c54089a28265aae9b4c088 |
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| 出典メモ | uspto-grants-1993_08 |
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