HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,2-Dichloroethane → 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)picolinamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,2-Dichloroethane | HCID 11 | — |
| Edukt | HOAt | HCID 181649 | — |
| Edukt | 3-Amino-4-chloropyridine | HCID 581932 | — |
| Edukt | 3-Amino-6-(2,6-difluorophenyl)picolinic acid | HCID 59226428 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 3-amino-N-(4-chloropyridin-3-yl)-6-(2,6-difluorophenyl)picolinamide | HCID 69042836 | 21% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08822497B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-99c3dfecc6454d368e50018cc0841db2 |
| Quellennotiz | uspto-grants-2014_09 |