反应详情

温度

40 °C

To a mixture of N-[1-amino-1-(4-{[(R)-[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 12b, 500 mg) and DMF (5 mL), carbonic acid 1-chloropropyl ester trans-2-fluorocyclohexyl ester (998 mg), sodium iodide (625 mg), and potassium hydrogen carbonate (100 mg) were added, and the resulting mixture was stirred at 40° C. for 76 hours. Water was added to the mixture, and the resulting mixture was extracted with ethyl acetate. The organic layer was sequentially washed twice with water and with saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was crudely purified by silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain a crudely purified product.

1. additionwere added
2. extractionthe resulting mixture was extracted with ethyl acetate
3. washThe organic layer was sequentially washed twice with water and with saturated aqueous sodium chloride solution
4. dry with materialdried 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 crudely purified by silica gel column chromatography (mixed solvent of methanol-ethyl acetate)
10. customto obtain a crudely purified product