関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Calcium Carbonate | HCID 10112 | — |
| 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 | Calcium | HCID 5460341 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Butyl Acetate | HCID 31272 | — |
| 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 (30.2 parts), ethyl bromocyanoacetate (38.4 parts), calcium carbonate (20 parts), copper catalyst, phase transfer catalyst and calcium or sodium chloride (each as indicated in the table below) and water (100 parts) is heated at 80° C. and held at 80° C. for 6 hours. The reaction mixture is cooled and stirred with water (100 parts), butyl acetate (100 parts by volume) and concentrated hydrochloric acid (100 parts by volume). The mixture is filtered and the residue is washed with butyl acetate (2×20 parts by volume). The filtrate and washes are combined and the butyl acetate layer is separated and washed with water (4×50 parts). The crude ethyl-1-cyano-3-(2',2'-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylate is isolated by removal of the butyl acetate under reduced pressure.
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-db4f54f5210949e58fe9a53847bdc973 |
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| 出典メモ | uspto-grants-1981_08 |
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