化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → 2'-Chloro-4'-(ethylthio)-5-(trifluoromethyl)-[1,1'-biphenyl]-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phosphine, tris(4-methylphenyl)- | HCID 13956 | — |
| 反応物 | (2-Hydroxy-5-(trifluoromethyl)phenyl)boronic acid | HCID 59436609 | — |
| 反応物 | 2-Chloro-4-(ethylthio)-1-iodo-benzene | HCID 67280185 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2'-Chloro-4'-(ethylthio)-5-(trifluoromethyl)-[1,1'-biphenyl]-2-ol | HCID 67281089 | — |
反応手順
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
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08158820B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-c914bdbf71e24bb585e2f0d95f4ed87d |
| 出典メモ | uspto-grants-2012_04 |