反应详情

To a solution of ethyl 3-oxo-3-(4-phenoxyphenyl)propionate (15 g, 52.8 mmol) in 1,2-dimethoxyethane (100 ml) was added sodium hydride (60% in oil, 2.11 g, 52.8 mmol) under ice-cooling, and the mixture was stirred at room temperature for 30 min. To the reaction solution was dropwise added a solution of 4-trifluoromethylbenzyl bromide (12.6 g, 52.8 mmol) in 1,2-dimethoxyethane (50 ml), and the mixture was stirred at room temperature for 4 hrs. The reaction solution was poured into water (200 ml) and extracted with ethyl acetate (200 ml×2). The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to give ethyl 3-oxo-3-(4-phenoxyphenyl)-2-((4-(trifluoromethyl)phenyl)methyl)propionate (15.4 g, 66%).

1. temperaturecooling
2. stirringthe mixture was stirred at room temperature for 4 hrs
3. extractionextracted with ethyl acetate (200 ml×2)
4. washThe extract was washed with water and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated under reduced pressure
7. customThe residue was recrystallized from ethyl acetate-hexane