関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Acrylonitrile | HCID 7855 | — |
| 反応物 | Octadecylamine | HCID 15793 | — |
| 反応物 | Azane;hydrate | HCID 12896473 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | n,n-Bis(2-cyanoethyl)octadecylamine | HCID 10872492 | — |
反応手順
40.2 g of acrylonitrile was added dropwise to an ethanol solution (150 ml) of 41.7 g of stearylamine at room temperature over 0.5 hours, 22.5 g of acetic acid was added dropwise thereto over 0.5 hours, and then stirred at 77° C. for 10 hours. After standing to cool to room temperature, the mixed solution was added with 200 ml of water and 22.8 g of 28% ammonia water, and extracted with 500 ml of ethyl acetate. The organic layer was separated from the solution, washed twice with 100 ml of water and 50 ml of saturated saline, dried over anhydrous magnesium sulfate. After distilling off the solvent, the concentrated residue was recrystallized using isopropyl alcohol as a solvent to obtain 42.4 g of a target compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08830811B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-d2fb62cec9164f48957a19e44449b09d |
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| 出典メモ | uspto-grants-2014_09 |
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