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Potassium Cyanide → 3-Chloro-5-(trifluoromethyl)pyridine-2-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | Fluoride Ion | HCID 28179 | — |
| 反応物 | 3-Chloro-2-fluoro-5-(trifluoromethyl)pyridine | HCID 1268075 | — |
| 触媒 | Trioctylmethylammonium chloride | HCID 21218 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Chloro-5-(trifluoromethyl)pyridine-2-carbonitrile | HCID 1473374 | 90% |
反応手順
A solution of potassium cyanide (71.6 g) in water (215 g) was added during 1 hour to a stirred mixture of 3-chloro-2-fluoro-5-trifluoromethylpyridine (199.5 g) and Aliquat 336 (tricaprylylmethylammonium chloride, 12.1 g) at 30° C. Stirring was maintained at this temperature for 4 hours at which time the amount of starting fluoride was less than 1% by hplc. The lower organic phase was separated and washed with aqueous sodium chloride solution and distilled to give 3-chloro-2-cyano-5-trifluoromethylpyridine (185.8 g, 90% yield) bp 90° C. at 15 mbar. The purity of this product was 98%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06921828B2 |
| 出典データセット | uspto-grants-2005_07 |
| ORD ID | ord-5972c1124d494dfca3add41c53cdbff2 |
| 出典メモ | uspto-grants-2005_07 |