反应详情

To a suspension of 5-bromouracil (5.0 g, 26 mmol) and potassium carbonate (7.2 g, 52 mmol) in N,N-dimethylformamide (25 mL) was added benzyl bromide (3.1 mL, 26 mmol) and the reaction mixture stirred 72 h. The reaction was treated with water (50 mL) and then extracted into ethyl acetate (3×75 mL). The aqueous layer was further extracted with dichloromethane (3×100 mL), the dichloromethane layers were combined, washed with water (2×50 mL), brine (1×50 mL), dried over magnesium sulfate, filtered and concentrated in vacuo. The resulting mixture of products was purified by pressurized silica gel chromatography (25% ethyl acetate in hexane) to provide 1-benzyl-5-bromo-1H-pyrimidine-2,4-dione.

1. extractionextracted into ethyl acetate (3×75 mL)
2. extractionThe aqueous layer was further extracted with dichloromethane (3×100 mL)
3. washwashed with water (2×50 mL), brine (1×50 mL)
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. additionThe resulting mixture of products
8. customwas purified by pressurized silica gel chromatography (25% ethyl acetate in hexane)