化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → Ethyl 5-Chloropyridine-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Bromo-5-chloropyridine | HCID 817098 | — |
| 反応物 | N,N-dimethylformamide ethanol | HCID 19794673 | — |
| 反応物 | HCID 178418416 | HCID 178418416 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| 生成物 | Ethyl 5-Chloropyridine-2-carboxylate | HCID 15414989 | — |
反応手順
Palladium acetate (117 mg), 1,1′-bis(diphenylphosphino)ferrocene (577 mg) and triethylamine (1.4 mL) were added to an ethanol-DMF mixed solvent (1/1, 30 mL) of 2-bromo-5-chloropyridine (1.0 g), and stirred overnight in a carbon monoxide atmosphere (1 atmospheric pressure) at 50° C. Ethanol was evaporated off under reduced pressure from the reaction solution, water was added to the resulting residue, and extracted with hexane/ethyl acetate (2/3). The organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated off under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=9/1 to 4/1) to obtain the entitled compound (1.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07566781B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-3357ba49289043cfb599c5ea7e8e0095 |
| 出典メモ | uspto-grants-2009_07 |