化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2-Bromo-6-methylpyridin-3-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Methyl-5-hydroxypyridine | HCID 14275 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-Bromo-6-methylpyridin-3-ol | HCID 11959101 | — |
反応手順
To a solution of 5-hydroxy-2-methylpyridine (Commercial, Aldrich, 44.5 g) in pyridine (400 ml) is added dropwise over 30 min at room temperature a solution of bromine (71.64 g) in pyridine (550 ml). The reaction mixture was stirred for an additional 1.5 h. The reaction mixture was poured into water (4 liters), stirred for a few minutes and extracted with diethyl ether (4×300 ml). The combined organics were dried over sodium sulphate and concentrated in vacuo to give a brown solid that was purified through silica using a 0-30% ethyl acetate in hexane system, to give the title compound as a beige solid, 37 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447074B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-f5e9f74c941d4f21b04a79c21b2e1bab |
| 出典メモ | uspto-grants-2016_09 |