関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Dichlorobenzonitrile | HCID 81051 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 3-Chloro-4-fluorobenzonitrile | HCID 145525 | 92% |
反応手順
172 g of 3,4-dichlorobenzonitrile, 200 g of dimethylsulfoxide, 69.6 g of potassium fluoride, and 3.95 g of (N,N-dimethylimidazolidino)tris-(diethylamino)phosphazenium chloride were placed in a 1 liter four-neck flask equipped with anchor stirrer, thermometer, and reflux condenser with bubble counter. The mixture was then heated with stirring to 170° C. and this temperature was maintained for 6 hours. The mixture was then cooled to room temperature, water was added to the reaction mixture in a volumetric ratio of 1:1, and the 3-chloro4-fluorobenzonitrile that precipitated was isolated by filtration, washing, and drying. 3-Chloro4-fluorobenzo-nitrile was obtained in a yield of 92% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07247733B2 |
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| 出典データセット | uspto-grants-2007_07 |
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| ORD ID | ord-f85aee8d23374cbdbccc03f44ec31822 |
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| 出典メモ | uspto-grants-2007_07 |
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