反应详情

温度

85 °C

Under nitrogen atmosphere, a mixture of acetic acid 2-{3-[(R)-{4-[amino(2-methylallyloxycarbonylimino)methyl]phenylamino}-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]-triazol-3-yl)methyl]-2-fluoro-5-methoxyphenoxyl}ethyl ester (1.0 g, 1.57 mmol), 3-methoxy-2,2-dimethylpropionic acid chloromethyl ester (598 mg, 3.31 mmol), rubidium carbonate (255 mg, 1.10 mmol), and N,N-dimethylacetamide (20 mL) was stirred at 85° C. for 75 minutes. After cooling to room temperature, ethyl acetate (100 mL) and water (100 mL) were added to the reaction mixture. The organic layer was collected, sequentially washed with water (100 mL) and saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain the captioned compound (560 mg) as a solid.

1. temperatureAfter cooling to room temperature
2. customThe organic layer was collected
3. washsequentially washed with water (100 mL) and saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationThe desiccant was filtered off
6. customthe filtrate obtained
7. concentrationwas concentrated under reduced pressure
8. customThe residue obtained
9. customwas purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate)