化工社化工社 化学情報印刷レポート · 研究参考用
Tetrahydrofuran → 3-Pyridinecarboxylic acid, 2-(4-methoxybenzoyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Furo[3,4-b]pyridine-5,7-dione | HCID 69688 | — |
| 反応物 | HCID 178491912 | HCID 178491912 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 3-Pyridinecarboxylic acid, 2-(4-methoxybenzoyl)- | HCID 11334368 | 27.8% |
反応手順
To a THF (15 ml) solution of pyridine-2,3-dicarboxylic acid anhydride (1.0 g, 6.7 mmol) was added dropwise a THF solution of 4-methoxyphenylmagnesium bromide (0.89M, 8.0 ml, 7.1 mmol) at -78° C. The reaction mixture was stirred at the same temperature for 1 h and then a saturated aqueous solution of NH4Cl (20 ml) was added to quench the reaction. The reaction mixture was diluted with 1N HCl and extracted with AcOEt. The organic layer was dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (E. Merck, Kieselgel 60/chloroform:methanol=10:1) to give 2-(4-methoxyphenylcarbonyl)-3-pyridine carboxylic acid (479 mg) as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05389620 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-b52f5b32182147ada5b88506affe7b8f |
| 出典メモ | uspto-grants-1995_02 |