関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propanal | HCID 527 | — |
| 反応物 | 3-Cyclopentene-1-acetaldehyde, 2,2,3-trimethyl- | HCID 98497 | — |
| 触媒 | Acetic Acid | HCID 176 | — |
| 触媒 | Piperidine | HCID 8082 | — |
| 生成物 | 2-Methyl-4-(2,2,3-trimethylcyclopent-3-en-1-yl)but-2-enal | HCID 3017557 | 80.6% |
反応手順
A 500 mL four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel was charged with 171 g (0.98 mol) of campholenic aldehyde (purity: 88%), 3.8 g (0.045 mol) of piperidine and 2.8 g (0.046 mol) of acetic acid, and the contents in the flask were stirred while heating at 100° C. Then, 92 g (1.6 mol) of propionaldehyde was gradually dropped into the flask for 6 h, and the resultant mixture was aged for 1 h and then cooled. Thereafter, 3.2 g (0.053 mol) of acetic acid was added to the mixture to remove amines therefrom, thereby separating the mixture into two layers. The thus separated organic layer was washed with water and separated into two layers, thereby obtaining 279 g (0.79 mol) of 2-methyl-4-(2,2,3-trimethylcyclopent-3-en-1-yl)-but-2-en-1-al (purity as measured by gas chromatography: 54.7%) (yield based on theoretical amount: 81%).
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-6ed8be084f0a4aabb4f5884d78af949f |
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| 出典メモ | uspto-grants-2010_06 |
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