関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Ethyl 2-(2,2-dichlorovinyl)-3,3-dimethyl-1-ethoxycarbonylcyclopropanecarboxylate | HCID 14914133 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Permethric acid | HCID 91658 | — |
反応手順
The mixture of ethyl 2-(2,2-dichlorovinyl)-3,3-dimethyl-1-ethoxycarbonylcyclopropanecarboxylate (1.5 g.) potassium hydroxide (2.0 g.) and ethanol (150 ml.) is refluxed for 2 hours, after which it is poured into water (500 ml.) and carefully acidified with concentrated hydrochloric acid. The white oily precipitate which is formed is collected by extraction with carbon tetrachloride, the extracts dried with anhydrous sodium sulphate, and the solvent evaporated under reduced pressure. The residual oil is heated under nitrogen to about 150°-160° C. for about 1.5 hours, and then cooled to form a crystalline mass. Recrystallisation from n-hexane yielded 2,2-dimethyl-3-(2,2-dichlorovinyl)cyclopropane carboxylic acid, m.p. 87°-90° C., believed to be principally the trans-isomer.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04257975 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-a4acd62499ac4d6cb313d58794d52ef5 |
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| 出典メモ | uspto-grants-1981_03 |
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