Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Carbonate → 2'-Chloro-4'-(ethylthio)-5-(trifluoromethyl)-[1,1'-biphenyl]-2-ol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Phosphine, tris(4-methylphenyl)- | HCID 13956 | — |
| 반응물 | (2-Hydroxy-5-(trifluoromethyl)phenyl)boronic acid | HCID 59436609 | — |
| 반응물 | 2-Chloro-4-(ethylthio)-1-iodo-benzene | HCID 67280185 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2'-Chloro-4'-(ethylthio)-5-(trifluoromethyl)-[1,1'-biphenyl]-2-ol | HCID 67281089 | — |
반응 단계
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
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08158820B2 |
| 출처 데이터셋 | uspto-grants-2012_04 |
| ORD ID | ord-c914bdbf71e24bb585e2f0d95f4ed87d |
| 출처 메모 | uspto-grants-2012_04 |