反应详情

温度

45 °C

Under nitrogen atmosphere, a mixture of isonicotinic acid 2-{3-[(4-{amino[benzoylimino]methyl}phenylamino)-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]-2-fluoro-5-methoxyphenoxy}ethyl ester (31.3 mg), 2,2-dimethylpropionic acid chloromethyl ester (9.1 mg), potassium hydrogen carbonate (6.7 mg), and DMF (2 mL) was stirred at 45° C. for 20 hours. The mixture was poured into ethyl acetate (100 mL) and water (20 mL). After shaking the mixture, the organic layer was collected, sequentially washed three times with water (20 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 (12.2 mg).

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