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Citric Acid → 3-Ethylsulfanyl pyridin-2-carboxylic acid [2-(2,2,2-trifluoroethyl)amino-5-trifluoromethylpyridin-3-yl]amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 3-(Ethylsulfanyl)pyridine-2-carboxylic acid | HCID 79006954 | — |
| 反応物 | N2-(2,2,2-trifluoroethyl)-5-trifluoromethylpyridine-2,3-diamine | HCID 86725179 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3-Ethylsulfanyl pyridin-2-carboxylic acid [2-(2,2,2-trifluoroethyl)amino-5-trifluoromethylpyridin-3-yl]amide | HCID 90324212 | 88.1% |
反応手順
A mixture of N2-(2,2,2-trifluoroethyl)-5-trifluoromethylpyridin-2,3-diamine (0.52 g), 3-ethylsulfanylpyridin-2-carboxylic acid (0.37 g), WSC (0.46 g), HOBt (27 mg) and pyridine (2 ml) was stirred at room temperature for 3 hours. To the reaction mixture was poured aqueous 10% citric acid solution, and then the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over sodium sulfate, and concentrated under reduced pressure to give 3-ethylsulfanyl pyridin-2-carboxylic acid [2-(2,2,2-trifluoroethyl)amino-5-trifluoromethylpyridin-3-yl]amide (0.75 g), which is hereinafter referred to as “intermediate compound (M3-43)”.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09120823B2 |
| 出典データセット | uspto-grants-2015_09 |
| ORD ID | ord-1225677c803d42a09aad29db42533660 |
| 出典メモ | uspto-grants-2015_09 |