関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Hydroxycitronellal | HCID 7888 | — |
| 反応物 | Dibutylamine | HCID 8148 | — |
| 反応物 | Hexanoic Acid | HCID 8892 | — |
| 生成物 | 3,7-Dimethyl-2-methylene-7-hydroxyoctanal | HCID 86632275 | 1,341.5% |
反応手順
A 3 L four-necked flask equipped with a stirrer, a thermometer and a reflux condenser was charged with 1032 g (6.0 mol) of hydroxycitronellal, 520 g (6.4 mol) of a 37% by mass formaldehyde aqueous solution, 53 g (0.41 mol) of dibutyl amine and 10 g (0.09 mol) of hexanoic acid, and the contents in the flask were stirred while heating at 95° C. After the elapse of 40 min, it was confirmed that no hydroxycitronellal was present in the raw mixture, and then the mixture was cooled and separated into two layers. The thus separated organic layer was subjected to distillation treatment, thereby obtaining 1058 g (5.5 mol) of 3,7-dimethyl-2-methylene-7-hydroxyoctanal (purity as measured by gas chromatography: 95%) (yield based on theoretical amount: 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732644B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-7f60cc2eaa174291a37a3a0e14fbbd2f |
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| 出典メモ | uspto-grants-2010_06 |
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