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HRID 856611作成日:2026年10月26日

Water → 2-(4-Fluoro-2-trifluoromethylbenzoyl)-4-methylpyridine

https://huagongshe.com/reaction/856611

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物2-Bromo-4-methylpyridineHCID 2734087—
反応物4-fluoro-N-methoxy-N-methyl-2-trifluoromethylbenzamideHCID 11218930—
反応物HCID 178418244HCID 178418244—
溶媒Diethyl EtherHCID 3283—
生成物2-(4-Fluoro-2-trifluoromethylbenzoyl)-4-methylpyridineHCID 2293852664.4%

反応条件

温度-78 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US07262185B2
出典データセットuspto-grants-2007_08
ORD IDord-470b42cc6f8a4141a1a69954747cd9e9
出典メモuspto-grants-2007_08