化工社化工社 化学情報印刷レポート · 研究参考用
Bromine → Ethyl 5-bromo-6-(5-chloro-2-thienyl)-6-oxohexanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | Ethyl 6-(5-chloro-2-thienyl)-6-oxohexanoate | HCID 18174688 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 5-bromo-6-(5-chloro-2-thienyl)-6-oxohexanoate | HCID 18174681 | 118.8% |
反応手順
Ethyl 6-(5-chloro-2-thienyl)-6-oxohexanoate (50.0 g) was dissolved in methylene chloride (150 ml), to which was added dropwise bromine (24.5 g) with stirring at room temperature. The mixture was stirred at room temperature for 1 hour, a 10% aqueous solution of sodium sulfite was then carefully added until disappearance of the red color of bromine, which was extracted with diethyl ether (200 ml×2). The organic layer was washed with a 10% aqueous solution of sodium hydrogen carbonate (100 ml), dried over anhydrous magnesium sulfate, and concentrated to give ethyl 5-bromo-6-(5-chloro-2-thienyl)-6-oxohexanoate as an oil (64.4 g, >99%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08067453B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-6aaca899621744af96f3a2ab3e9050ca |
| 出典メモ | uspto-grants-2011_11 |