関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 3-(2,2-Dichloroethenyl)-2,2-dimethylcyclopropane-1-carbonitrile | HCID 12898173 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Cyclopropanecarboxylic acid, 3-(2,2-dichloroethenyl)-2,2-dimethyl-, ethyl ester | HCID 101094 | 92.4% |
反応手順
The procedure described in Example 2 is repeated up to the point at which the mixture of 1-cyano-3-(2',2'-dichlorovinyl)-2,2-dimethylcyclopropane, sulphuric acid and water has been heated and stirred at 80° C. for 6 hours and then cooled below 30° C. 16 Parts of ethanol are added to the reaction mixture below 50° C. The mixture is then heated at 100° C. for a further 12 hours, cooled to 20° C. and drowned into 100 parts of water. The aqueous mixture is extracted with toluene (2×50 parts), the toluene extracts are combined and the solvent is removed by evaporation under reduced pressure. There are obtained 17.6 parts of ethyl 3-(2',2'-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylate as a brown oil containing 40.4% of the cis-isomer and 21.8% of the trans-isomer. The overall yield is 92.4%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04236018 |
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| 出典データセット | uspto-grants-1980_11 |
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| ORD ID | ord-46720017eb7d4bcf80f5d3cbefa631db |
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| 出典メモ | uspto-grants-1980_11 |
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