化工社化工社 化学情報印刷レポート · 研究参考用
N-bromobutanimide → 1,5-Dibromo-2,4-difluorobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 1-Bromo-2,4-difluorobenzene | HCID 67674 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 1,5-Dibromo-2,4-difluorobenzene | HCID 10564511 | 96.9% |
反応手順
Under ice cooling, a solution of 25.35 g of 1-bromo-2,4-difluorobenzene in 100 mL of concentrated sulfuric acid was added with 25.7 g of N-bromosuccinimide, and stirred for 30 minutes at this temperature and for 2 days at room temperature. After cooling on ice, the reaction solution was added with ice, and extracted with 300 mL of diethyl ether. The organic layer was successively washed with water, saturated aqueous sodium hydrogen carbonate and saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resulting crude product was purified and separated by silica gel column chromatography (n-hexane), to afford 34.6 g of the title compound as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429609B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-212fd29e870144d78e5e3e6f181494d7 |
| 出典メモ | uspto-grants-2008_09 |