関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | 2,4-Dichlorophenylacetonitrile | HCID 80566 | — |
| 生成物 | 2-(2,4-Dichlorophenyl)-3-hydroxyprop-2-enenitrile | HCID 1483069 | 74.1% |
反応手順
0.6 g of metal sodium was added to dry ethanol to obtain an ethanol solution of sodium ethoxide. Then, a mixed liquid comprising 37.2 g of 2,4-dichlorophenyl acetonitrile and 22.2 g of ethyl formate, was added thereto under heating to 70° C. After the addition, the mixture was further heated and refluxed for 2 hours and then, left to stand for 1 day. The reaction solution was cooled to 0° C. and then subjected to filtration. After washing with diethyl ether, the sodium salt collected by filtration was added to 130 ml of distilled water, and 9 ml of acetic acid was dropwise added thereto under cooling at 0° C. After the dropwise addition, the mixture was stirred at room temperature for about 30 minutes. Then, the formed precipitate was collected by filtration and washed with water. It was dried to obtain 31.7 g (yield: 74%) of the desired product. Melting point: 162-163° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06048823 |
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| 出典データセット | uspto-grants-2000_04 |
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| ORD ID | ord-11e78bae281a4e05be45e16ffb7e34a9 |
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| 出典メモ | uspto-grants-2000_04 |
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