関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Amino-6-(trifluoromethyl)pyridine | HCID 821024 | — |
| 反応物 | 3-Chloropyridine-2-carboxylic acid | HCID 824632 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3-chloro-N-(6-trifluoromethylpyridin-2-yl)picolinamide | HCID 118113287 | 89.1% |
反応手順
A mixture of 0.81 g of 2-amino-6-trifluoromethylpyridine, 0.78 g of 3-chloropicolinic acid, 1.15 g of EDCI hydrochloride, 0.06 g of HOBt and 10 mL of pyridine was stirred at 70° C. for 2 hours. A saturated aqueous sodium bicarbonate solution was poured to the cooled reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure, and the resulting solid was washed with hexane and dried to obtain 1.33 g of 3-chloro-N-(6-trifluoromethylpyridin-2-yl)picolinamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09185910B2 |
|---|
| 出典データセット | uspto-grants-2015_11 |
|---|
| ORD ID | ord-135b62c9e8eb46e3957a6bc97a77bb43 |
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| 出典メモ | uspto-grants-2015_11 |
|---|
