化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Nitrate → 5-Bromo-6-fluoro-8-nitroquinaldine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 反応物 | 5-Bromo-6-fluoro-2-methylquinoline | HCID 13035313 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Bromo-6-fluoro-8-nitroquinaldine | HCID 13191962 | 91.8% |
反応手順
A solution of 11.5 g of potassium nitrate in 30 ml of concentrated sulfuric acid was added to 21.0 g of 5-bromo-6-fluoroquinaldine in 117 ml of concentrated sulfuric acid dropwise at -5° C. After stirring at room temperature for 5 hours, the reaction mixture was poured into 2 l of ice water to precipitate solids which were then collected by filtration. The filtrate was rendered alkaline to form a small amount of solids, which together with the former solids were dissolved in dichloromethane. After the solution was dried over sodium sulfate the solvent was distilled off. Recrystallization of the residue from isopropanol gave 22.9 g of 5-bromo-6-fluoro-8-nitroquinaldine. m.p. 135°-137° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04399134 |
| 出典データセット | uspto-grants-1983_08 |
| ORD ID | ord-3ce4858b3b4c477693aa3864b68984a6 |
| 出典メモ | uspto-grants-1983_08 |