Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)picolinamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | HOAt | HCID 181649 | — |
| 반응물 | 3-Amino-4-chloropyridine | HCID 581932 | — |
| 반응물 | 3-Amino-6-(2,6-difluorophenyl)picolinic acid | HCID 59226428 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)picolinamide | HCID 69042836 | 21% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822497B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-99c3dfecc6454d368e50018cc0841db2 |
| 출처 메모 | uspto-grants-2014_09 |