反应详情

To a mixture of 2-bromopropiophenone (2.13 g), 2,6-difluorophenylacetic acid (1.81 g) and acetonitrile (25 mL), triethylamine (1.52 g) was added dropwise in a water bath, stirred at room temperature for 4 hours and then allowed to stand still overnight. To the mixture, 4.57 g of 1,8-diazabicyclo[5.4.0]-7-undecene (hereinafter, referred to as DBU) was added dropwise under ice cooling. The mixture was stirred at room temperature for one hour. Thereafter, to the obtained mixture, air was blown in while stirring at room temperature for 5 hours. To the reaction mixture, ice and 1 mol/L hydrochloric acid were added. The mixture was extracted with ethyl acetate. The organic layer was sequentially washed with a saturated aqueous sodium bicarbonate solution and a saturated saline solution, dried over an anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 3-(2,6-difluorophenyl)-5-hydroxy-5-methyl-4-phenyl-2(5H)-furanone (2.83 g).

1. additionwas added dropwise in a water bath
2. waitto stand still overnight
3. additionwas added dropwise under ice cooling
4. stirringThe mixture was stirred at room temperature for one hour
5. stirringwhile stirring at room temperature for 5 hours
6. extractionThe mixture was extracted with ethyl acetate
7. washThe organic layer was sequentially washed with a saturated aqueous sodium bicarbonate solution
8. dry with materiala saturated saline solution, dried over an anhydrous magnesium sulfate
9. concentrationconcentrated under reduced pressure