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Acetic Acid → 2-Ethylhexyl 3-(4-aminophenyl)-2-cyanoacrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | 4-Aminobenzaldehyde | HCID 11158 | — |
| 反応物 | 2-Ethylhexyl cyanoacetate | HCID 96359 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-Ethylhexyl 3-(4-aminophenyl)-2-cyanoacrylate | HCID 53851611 | 66.1% |
反応手順
36.3 g (0.3 mol) of p-aminobenzaldehyde are suspended in 450 ml of isopropanol. A mixture of 59.1 g (0.3 mol) of 2-ethylhexyl cyanoacetate and of catalyst (0.375 ml of diethylamine and 1.125 ml of acetic acid) is introduced therein. The mixture is refluxed for 5 hours. The same amount of catalyst is added again and refluxing is continued for a further 4 hours. The insoluble materials are removed by hot filtration and the mixture is concentrated to a volume of 300 ml and left to crystalize. After filtration and drying, 59.6 g (66% yield) of an orange-coloured powder are obtained, and are used without further purification for the following step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07390916B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-241a139bf82a4c8981d30fdba0222782 |
| 出典メモ | uspto-grants-2008_06 |