反应详情

温度

50 °C

A mixture of N-[1-amino-1-[4-({(5-chloromethoxy-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}amino)phenyl]methylidene]benzamide (500 mg), 2,2-dimethylmalonic acid mono-(2,2-dimethylpropyl)ester (1.56 g), sodium iodide (1.16 g), potassium hydrogen carbonate (543 mg), and DMA (50 mL) was stirred at 50° C. for 7 hours. After cooling the mixture to room temperature, ethyl acetate was added thereto, and the resulting mixture was sequentially washed twice with water and with 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 NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (500 mg).

1. temperatureAfter cooling the mixture to room temperature
2. washthe resulting mixture was sequentially washed twice with water and with saturated aqueous sodium chloride solution
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationThe desiccant was filtered off
5. customthe filtrate obtained
6. concentrationwas concentrated under reduced pressure
7. customThe residue obtained
8. customwas purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate)