関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Bromo-4-methylpyridine | HCID 2734087 | — |
| 反応物 | 4-fluoro-N-methoxy-N-methyl-2-trifluoromethylbenzamide | HCID 11218930 | — |
| 反応物 | HCID 178418244 | HCID 178418244 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(4-Fluoro-2-trifluoromethylbenzoyl)-4-methylpyridine | HCID 22938526 | 64.4% |
反応手順
2-bromo-4-methylpyridine (4.7 g) was dissolved in diethylether (150 ml), and the mixture was cooled to −78° C. under argon atmosphere. 1.6M n-butyllithium hexane solution (16.8 ml) was added dropwise to the solution, and the mixture was stirred for 30 minutes. The reaction solution was added dropwise to a solution of 4-fluoro-N-methoxy-N-methyl-2-trifluoromethylbenzamide (6.2 g) in diethylether (50 ml) under argon atmosphere at −78° C. The mixture was allowed to be at room temperature and stirred overnight, and water was added to the mixture. The mixture was concentrated and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane), to give 2-(4-fluoro-2-trifluoromethylbenzoyl)-4-methylpyridine (4.5 g) as pale yellow amorphous.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07262185B2 |
|---|
| 出典データセット | uspto-grants-2007_08 |
|---|
| ORD ID | ord-470b42cc6f8a4141a1a69954747cd9e9 |
|---|
| 出典メモ | uspto-grants-2007_08 |
|---|