反应详情

温度

60 °C

A mixture of 7-(methylthio)-1H-pyrazolo[4,3-d]pyrimidine (747 mg), 2-{2-[(methylsulfonyl)oxy]ethoxy}ethyl benzoate (1.43 g), potassium carbonate (931 mg) and N,N-dimethylformamide (12 mL) was stirred at 60° C. for 4 hrs. The reaction mixture was poured into water (30 mL), and the mixture was extracted with ethyl acetate (50 mL×2). The organic layers were combined, washed with saturated brine and dried over anhydrous magnesium sulfate. After concentration under reduced pressure, the residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=80:20→20:80), and further purified by basic silica gel column chromatography (eluent, hexane:ethyl acetate=90:10→40:60) to give the title compound (533 mg).

1. extractionthe mixture was extracted with ethyl acetate (50 mL×2)
2. washwashed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationAfter concentration under reduced pressure
5. customthe residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=80:20→20:80)
6. customfurther purified by basic silica gel column chromatography (eluent, hexane:ethyl acetate=90:10→40:60)