反应详情

Benzimidazole (0.395 g) and potassium carbonate (1 g) were added to a stirred solution of 6-(chloromethyl)-3-methyl-1-(1-methylethyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (0.55 g) in anhydrous dimethylformamide (5 ml) at room temperature. After 2 days, water (50 ml) was added and the mixture was extracted with ethyl acetate (2×50 ml). The organic extracts were dried over anhydrous magnesium sulfate and filtered through a silica pad which was washed with ethyl acetate. The filtrate was evaporated and the residue was purified twice by normal-phase preparative HPLC with gradient dichloromethane/ethanol elution to give the title compound (0.394 g) as a foam.

1. extractionthe mixture was extracted with ethyl acetate (2×50 ml)
2. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
3. filtrationfiltered through a silica pad which
4. washwas washed with ethyl acetate
5. customThe filtrate was evaporated
6. customthe residue was purified twice by normal-phase preparative HPLC with gradient dichloromethane/ethanol elution