化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)picolinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | 3-Amino-4-chloropyridine | HCID 581932 | — |
| 反応物 | 3-Amino-6-(2,6-difluorophenyl)picolinic acid | HCID 59226428 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)picolinamide | HCID 69042836 | 21% |
反応手順
A solution of 3-amino-6-(2,6-difluorophenyl)picolinic acid (1.0 equiv.), 4-chloropyridin-3-amine (2.0 equiv.), HOAt (1.0 equiv.), and EDC (1.0 equiv.) in DCM at a concentration of (0.2M) was stirred for 24 hr. Water was added to the reaction, followed by EtOAc. The organic layer was separated, dried with brine, MgSO4, and concentrated. The crude material was purified via SiO2 column chromatography eluting with EtOAc and hexanes (1:1) to give the product as a light yellow solid (21% yield). LCMS (m/z): 361.1 (MH+); LC Rt=3.28 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-99c3dfecc6454d368e50018cc0841db2 |
| 出典メモ | uspto-grants-2014_09 |