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 (Example 1a, 45 mg) and DMF (2 mL), cesium carbonate (29 mg) and 3-methoxy-2,2-dimethylpropionic acid chloromethyl ester (20 mg) were sequentially added, and the resulting mixture was stirred at 60° C. for 4 hours. The resulting mixture was poured into ethyl acetate (30 mL) and water (20 mL). After shaking the mixture, the organic layer was collected. The organic layer was sequentially washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (20 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (20 mg).

1. additionwere sequentially added
2. stirringAfter shaking the mixture
3. customthe organic layer was collected
4. washThe organic layer was sequentially washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (20 mL)
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe resulting mixture was filtered
7. customthe filtrate obtained
8. concentrationwas concentrated under reduced pressure
9. customThe residue obtained
10. customwas purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate)