化工社化工社 化学情報印刷レポート · 研究参考用
2-Chloropyridin-4-amine → 3-Bromo-2-chloropyridin-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloropyridin-4-amine | HCID 84432 | — |
| 反応物 | N-Bromosuccinamide | HCID 9834204 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3-Bromo-2-chloropyridin-4-amine | HCID 29919300 | — |
反応手順
4-amino-2-chloropyridine (50 g, 388 mmol) was dissolved in glacial acetic acid (500 mL). To this solution was added N-bromosuccinamide (75 g, 426 mmol,) portionwise at room temperature (water bath cooling was provided to control the exothermicity). The reaction mixture was stirred at RT for 1 h at which point the reaction was found complete (as monitored by TLC). Solvent was removed under reduced pressure followed by azeotropic distillation with ethanol. The crude product was purified by column chromatography on silica gel (230-400 mesh) eluting with ethyl acetate hexane mixture.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198448B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-f49c884ff4b54645b8e49b4da4d9151a |
| 出典メモ | uspto-grants-2012_06 |