反应详情

温度

60 °C

500 mg (2.71 mmol) of 4,7-difluoro-1H-isoindole-1,3(2H)-dione and 889.7 mg (2.71 mmol) of cesium carbonate were added to a solution of 964.7 mg (2.71 mmol) of tert-butyl(+/−)-[4-(bromomethyl)phenyl](cyclopentyl)acetate in 2 ml of DMF. The mixture was stirred at 60° C. for 2 h, and the reaction mixture was then added to ice-water. The mixture was extracted three times with ethyl acetate. The combined organic phases were washed with saturated sodium chloride solution and dried over magnesium sulfate. The crude product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 10:1 to 5:1). This gave 424 mg (34.1% of theory) of the target compound.

1. extractionThe mixture was extracted three times with ethyl acetate
2. washThe combined organic phases were washed with saturated sodium chloride solution
3. dry with materialdried over magnesium sulfate
4. customThe crude product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 10:1 to 5:1)