反应详情

温度

60 °C

To a solution of 3-(4-hydroxy-2-methyl-6-oxo-6H-pyrimidin-1-yl)-4-methyl-benzoic acid methyl ester from Step D (800 mg, 66% purity, 1.93 mmol) in N,N-dimethylformamide (3 mL) was added 4-methoxybenzyl chloride (0.26 mL, 1.93 mmol), potassium carbonate (666 mg, 4.82 mmol) and 18-crown-6 (80 mg). The slurry was heated at 60° C. for two hours. The solution was allowed to cool to ambient temperature and was partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over magnesium sulfate. The slurry was filtered and concentrated to a brown oil. Normal phase chromatography (ethyl acetate/heptane) provided the alkylated product as a white solid (170 mg, 22% yield). MS (M+H): 395

1. temperatureto cool to ambient temperature
2. customwas partitioned between ethyl acetate and water
3. washThe organic layer was washed with water and brine
4. dry with materialdried over magnesium sulfate
5. filtrationThe slurry was filtered
6. concentrationconcentrated to a brown oil