関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propionitrile | HCID 7854 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | 2,3-Dichloro-5-(trifluoromethyl)pyridine | HCID 112234 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Chloro-5-(trifluoromethyl)pyridine-2-carbonitrile | HCID 1473374 | 73% |
反応手順
Propionitrile (656 ml), 2,3-dichloro-5-trifluoromethylpyridine (87.5 g) and 4-dimethylaminopyridine (52 g) were heated at reflux for 5 hours under nitrogen. The mixture was cooled and a solution of sodium cyanide (30 g) in water (110 ml) added at 15° C. After stirring at 15° C. for 5 hours the reaction was complete and water (250 ml) added to dissolve the inorganic salts. The organic phase was washed with water followed by extraction with 2N HCl to remove 4-dimethylaminopyridine. Propionitrile was removed by vacuum distillation at 40° C. to give the product, 3-chloro-2-cyano-5-trifluoromethylpyridine in 73 to 84% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06699993B1 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-2759955b5a064331b73b1134fed2a2e3 |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|