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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)-5-fluoropicolinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | 3-Amino-4-chloropyridine | HCID 581932 | — |
| 反応物 | 3-Amino-6-(2,6-difluorophenyl)-5-fluoropicolinic acid | HCID 59226513 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)-5-fluoropicolinamide | HCID 69041531 | 14% |
反応手順
To a solution of 4-chloropyridin-3-amine (1.0 equiv.) and 3-amino-6-(2,6-difluorophenyl)-5-fluoropicolinic acid (1.0 equiv.) in NMP (1 M) was added HOAt and EDCI sequentially. The reaction mixture was stirred at room temperature for 2 days. The crude reaction was purified by prep HPLC to give 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)-5-fluoropicolinamide (14%). LCMS (m/z): 379.0 (MH+); LC Rt=3.49 min
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822497B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-c2a9a24737da4afeb34ee92ab5fc4609 |
| 出典メモ | uspto-grants-2014_09 |