化工社化工社 化学情報印刷レポート · 研究参考用
Sulfuric Acid → Ethyl 2-bromoisonicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 2-Bromoisonicotinic acid | HCID 222701 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 2-bromoisonicotinate | HCID 3847769 | — |
反応手順
To a suspension of 2-bromo4-pyridine carboxylic acid (prepared according to the method of Ashimori, Chem. Pharm. Bull. 38 (9) 2446-2458 (1990)) in 2:1 toluene: absolute ethanol (45 mL) was added sulfuric acid (0.75 mL). The mixture was heated at reflux for 16 h. The mixture was poured into saturated aqueous sodium bicarbonate and extracted with chloroform (3 times). The combined chloroform extracts were dried over magnesium sulfate, filtered and concentrated afforded the crude product as a yellow oil. Purification by silica gel chromatography eluting with 9:1 hexane:ethyl acetate to afford the title compound (900 mg) as a clear, colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06251925B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-87d436ec62d7494299d612f339bfac85 |
| 出典メモ | uspto-grants-2001_06 |