関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichlorofluoromethane | HCID 6370 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 1-Hexene, 2-ethoxy- | HCID 10376321 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-Butyl-2-chloro-1-ethoxy-2-fluorocyclopropane | HCID 12786235 | — |
反応手順
To a solution of 61.0 g. of 2-ethoxy-1-hexene, 135 ml. of 13.5 M potassium hydroxide and 217 g. of "18-crown -6" ether at -15° C. is added dropwise over 30 minutes at 0°, a 90 ml. portion of dichlorofluoromethane. After the addition, the mixture is placed in an ice bath. An exotherm raises the temperature to 20° C., whereupon the mixture is placed in a dry-ice/carbon tetrachloride bath to maintain the temperature at -5° C. to 0° C. After three hours at this temperature, the reaction mixture is diluted with water and extracted with ether. The ether extracts are combined, washed with water, then brine, dried over potassium carbonate and concentrated in vacuo to an oil. This oil is distilled through a 6 inch Vigreux column to provide 82 g. of the desired compound as a colorless liquid, b.p. 70°-71° C., 16 mm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04297516 |
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| 出典データセット | uspto-grants-1981_10 |
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| ORD ID | ord-64a44d5f3cc143a290d2f0f98e68c855 |
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| 出典メモ | uspto-grants-1981_10 |
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