関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Isonicotinic Acid | HCID 5922 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 3-Amino-5-(trifluoromethyl)-1,2-dihydropyridin-2-one | HCID 2315787 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178522158 | HCID 178522158 | 76.9% |
反応手順
A mixture of 1.0 g of 3-amino-2-hydroxy-5-trifluoromethylpyridine, 0.69 g of isonicotinic acid, 1.40 g of WSC and 7 ml of pyridine was stirred while heating at 80° C. for two hours. The reaction mixture was cooled to room temperature, and then water was added to the reaction mixture, followed by extraction with ethyl acetate three times. The combined organic layers were washed with water and a saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 1.22 g of N-[2-hydroxy-5-(trifluoromethyl)pyridin-3-yl]isonicotinamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08324387B2 |
|---|
| 出典データセット | uspto-grants-2012_12 |
|---|
| ORD ID | ord-54e2c24f77ac4e0b8b9480e0c993d58a |
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| 出典メモ | uspto-grants-2012_12 |
|---|
