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Water → 3-Chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 3-chloro-5-(trifluoromethyl)pyridine-2-carboxylate | HCID 22013558 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid | HCID 2821908 | 84.5% |
反応手順
423 g of ethyl 3-chloro-5-trifluoromethyl-2-pyridinecarboxylate (Example H2) is initially introduced into a mixture of 800 ml of water and 160 ml of ethanol. 800 ml of a 2N sodium hydroxide solution are added dropwise at a temperature below 35° C. After 3 hours, the mixture is washed twice with methylene chloride and then rendered acid with an excess of concentrated hydrochloric acid, while cooling in an ice-bath. The slurry formed is filtered and the solid is washed with water and dried in vacuo. 318 g of the desired product are obtained as a white solid of melting point 135° C. (decomposition).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06204221B1 |
| 出典データセット | uspto-grants-2001_03 |
| ORD ID | ord-f64f025ff8dd4437abebd97f4a7fdd47 |
| 出典メモ | uspto-grants-2001_03 |