反应详情

温度

60 °C

To a mixture of N-[1-amino-1-(4-{[[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}phenyl)methylidene]benzamide (120 mg) and DMF (3 mL), potassium hydrogen carbonate (30 mg) and 3-methoxymethoxy-2,2-dimethylpropionic acid chloromethyl ester (54.8 mg) were sequentially added, and the resulting mixture was stirred at 60° C. for 14 hours. To the mixture, ethyl acetate (100 mL) was added. The resulting mixture was sequentially washed three times with water (50 mL) and with saturated aqueous sodium chloride solution (50 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered and the obtained filtrate was concentrated under reduced pressure. The obtained residue was purified by NAM silica gel column chromatography (mixed solvent of heptane-ethyl acetate and methanol-ethyl acetate) to obtain the captioned compound (40 mg).

1. additionwere sequentially added
2. washThe resulting mixture was sequentially washed three times with water (50 mL)
3. dry with materialwith saturated aqueous sodium chloride solution (50 mL), and dried over anhydrous magnesium sulfate
4. filtrationThe resulting mixture was filtered
5. concentrationthe obtained filtrate was concentrated under reduced pressure
6. customThe obtained residue was purified by NAM silica gel column chromatography (mixed solvent of heptane-ethyl acetate and methanol-ethyl acetate)