反应详情

温度

45 °C

To a mixture of [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]carbamic acid 2,2-dimethylpropyl ester (Example 2b, 70 mg), potassium hydrogen carbonate (74 mg), and DMF (5 mL), sodium iodide (79 mg) and 2,2-dimethylmalonic acid monoisopropyl ester [CAS No. 7695-26-3] (92 mg) were added, and the resulting mixture was stirred at 45° C. overnight. The reaction 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 a racemate of the captioned compound.

1. addition7695-26-3] (92 mg) were added
2. filtrationThe reaction mixture was filtered
3. customthe filtrate obtained
4. concentrationwas concentrated under reduced pressure
5. customThe residue obtained
6. customwas purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate)
7. customto obtain a racemate of the captioned compound