反应详情

温度

120 °C

A mixture of 2-methylimidazole (50 g, 0.6 mol), ethyl 4-fluorobenzoate (100 g, 0.6 mol) and potassium carbonate (415 g, 3 mol) in dry DMSO (1.5 l ) was heated at 120° C. for 66 hours under a nitrogen atmosphere. After cooling to room temperature, the reaction mixture was poured into ice-cold water (1 l ), and extracted with Et2O (750 ml×2). The organic phase was washed with water (500 ml) and brine (500 ml), dried over MgSO4 and evaporated. The residual solid was recrystallized from ethyl acetate-hexane to give the titled compound (47 g, 33%) as yellow needles.

1. temperatureAfter cooling to room temperature
2. extractionextracted with Et2O (750 ml×2)
3. washThe organic phase was washed with water (500 ml) and brine (500 ml)
4. dry with materialdried over MgSO4
5. customevaporated
6. customThe residual solid was recrystallized from ethyl acetate-hexane