HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → 2'-Chloro-4'-(ethylthio)-5-(trifluoromethyl)-[1,1'-biphenyl]-2-ol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Phosphine, tris(4-methylphenyl)- | HCID 13956 | — |
| Edukt | (2-Hydroxy-5-(trifluoromethyl)phenyl)boronic acid | HCID 59436609 | — |
| Edukt | 2-Chloro-4-(ethylthio)-1-iodo-benzene | HCID 67280185 | — |
| Katalysator | palladium(II) acetate | HCID 167845 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 2'-Chloro-4'-(ethylthio)-5-(trifluoromethyl)-[1,1'-biphenyl]-2-ol | HCID 67281089 | — |
Reaktionsschritte
A mixture of palladium acetate (0.045 g) and tri-p-tolylphosphine (0.213 g) in methanol (10 ml) was stirred at RT for 30 min. The product from step (iii) (1 g), sodium carbonate (1.27 g), the product from example (26) step (i) (1.19 g) and methanol (20 ml) were added and the mixture heated under reflux for 6 h. The solvent was removed under reduced pressure and the residue partitioned between diethylether and 2M hydrochloric acid. The organics were separated, dried and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with 10% ethylacetate/isohexane. Yield 0.503 g
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08158820B2 |
| Quelldatensatz | uspto-grants-2012_04 |
| ORD ID | ord-c914bdbf71e24bb585e2f0d95f4ed87d |
| Quellennotiz | uspto-grants-2012_04 |