関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 3-Chloropyridine-4-carboxylic acid | HCID 2735816 | — |
| 反応物 | 2-Amino-4-chloro-5-(trifluoromethyl)phenol | HCID 66880478 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-chloro-N-[5-chloro-2-hydroxy-4-trifluoromethylphenyl]isonicotinamide | HCID 66880791 | 69.9% |
反応手順
A mixture of 0.60 g of 2-amino-4-chloro-5-trifluoromethylphenol, 0.43 g of 3-chloroisonicotinic acid, 0.67 g of WSC and 5 ml of pyridine was stirred while heating at 80° C. for three hours. The reaction mixture was cooled to room temperature, and then water was added, followed by extraction with ethyl acetate three times. The combined organic layers were washed with water and a saturated sodium chloride solution, dried anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.67 g of 3-chloro-N-[5-chloro-2-hydroxy-4-trifluoromethylphenyl]isonicotinamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08242133B2 |
|---|
| 出典データセット | uspto-grants-2012_08 |
|---|
| ORD ID | ord-729614d889394d2598aae2e6066655e1 |
|---|
| 出典メモ | uspto-grants-2012_08 |
|---|
