化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → 5-Bromo-2-(3,4-difluorophenyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2,5-Dibromopyridine | HCID 69353 | — |
| 反応物 | 3,4-Difluorophenylboric acid | HCID 21869672 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 5-Bromo-2-(3,4-difluorophenyl)pyridine | HCID 19386419 | — |
反応手順
A mixture of 6.2 g of 3,4-difluorophenylboric acid, 8.5 g of 2,5-dibromopyridine, 0.31 g of tetrakistriphenylphosphine palladium, 60 ml of ethanol, 120 ml of benzene and 120 ml of 2N sodium carbonate solution is heated to boiling (66° C.) for 7 hours while stirring. After cooling the mixture is extracted with diethyl ether. The organic phase is washed with 100 ml of saturated sodium hydrogen carbonate solution and 100 ml of water, dried over sodium sulphite, filtered and concentrated. Purification of the residue by chromatography on silica gel with hexane/ethyl acetate 19:1 yields pure 5-bromo-2-(3,4-difluorophenyl)pyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05292452 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-43a88de3b9ea44f4b68b91b7d90f87be |
| 出典メモ | uspto-grants-1994_03 |