化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → 4-[2-(4-Fluorophenyl)ethyl]-2-(4-methoxybenzyloxy)-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-Fluorostyrene | HCID 67883 | — |
| 反応物 | 9-Borabicyclo(3.3.1)nonane | HCID 78966 | — |
| 反応物 | 4-[(e)-2-(4-Fluorophenyl)vinyl]-1-{4-[2-(1-pyrrolidinyl)ethoxy]phenyl}-1h-pyridin-2-one | HCID 11188891 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 4-[2-(4-Fluorophenyl)ethyl]-2-(4-methoxybenzyloxy)-pyridine | HCID 68431108 | 100% |
反応手順
9-Borabicyclo[3.3.1]nonane (540 mg) was added to THF solution (5 mL) of 4-fluorostyrene (240 mL) and stirred at room temperature for 2 hours. To the reaction liquid, the compound synthesized in Step (1) of Example 45(340 mg), tetrakis(triphenylphosphine)palladium (60 mg), DMF (5 mL) and 2M aqueous sodium carbonate solution (1 mL) were added and stirred at 100° C. for 19 hours. Saturated brine was added to the reaction liquid, followed by extraction with ethyl acetate and drying over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the residue was purified on silica gel column chromatography (C-200; ethyl acetate:hexane=1:9-1:4) to provide the title compound (336 mg, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732456B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-176101cd28c147d0814db60ad04c21e6 |
| 出典メモ | uspto-grants-2010_06 |