関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 2-bromo-2-cyanoacetate | HCID 14469 | — |
| 反応物 | 1,3-Pentadiene, 1,1-dichloro-4-methyl- | HCID 108746 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Ethyl 1-cyano-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylate | HCID 12898169 | — |
反応手順
A mixture of 1,1-dichloro-4-methylpenta-1,3-diene (15.1 parts), copper-containing catalyst in amount indicated in the table below and methanol (32 parts) is heated to reflux and ethyl bromocyanoacetate (19.2 parts) in methanol (14 parts) is then added at a uniform rate during 6 hours, and the acid-base balance ("pH" as indicated by a pH meter) is maintained at a predetermined value by the addition of a 13% solution of sodium methoxide in methanol. On completion of the ethyl bromocyanoacetate addition, heating at reflux temperature is continued for a further 2 hours, maintaining the desired acid-base balance as necessary. The resulting solution is evaporated under reduced pressure to remove the solvent and the product is isolated as described in Examples 2-6 above. The yield, strength and composition of the ethyl 1-cyano-3-(2',2'-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylate obtained are given in the following table together with other reaction details:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04284582 |
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| 出典データセット | uspto-grants-1981_08 |
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| ORD ID | ord-71b6c52dd9ca4d3c8b4947c4d18a9a48 |
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| 出典メモ | uspto-grants-1981_08 |
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