関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | 1-Chloro-2-methyl-3-prop-2-enylbenzene | HCID 10678653 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 1-Cyano-2-methyl-3-prop-2-enylbenzene | HCID 19786485 | 50.9% |
反応手順
30 g of 1-chloro-2-methyl-3-prop-2-enylbenzene are dissolved in 150 ml of N-methylpyrrolidone, and 25 g of copper(I) cyanide are added. The reaction mixture is heated at 190° C. for 30 hours while stirring. After the mixture has been cooled to 20° C., 125 ml of ethylenediamine and 300 ml of water are added. Stirring is then carried out for 1 hour at 50° C. and for 14 hours at 20° C. Working up is effected by extracting with diethyl ether, washing the organic phase and drying over sodium sulfate, removing the drying agent and distilling off the organic solvent. 24.5 g of crude product are obtained. After chromatography (silica gel/toluene), 14.4 g of pure 1-cyano-2-mehtyl-3-prop-2-enylbenzene are isolated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05256666 |
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| 出典データセット | uspto-grants-1993_10 |
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| ORD ID | ord-a303102d4c8248989303cabd7d70b551 |
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| 出典メモ | uspto-grants-1993_10 |
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