反应详情

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, 80 mg) and DMF (5 mL), sodium iodide (183 mg), potassium hydrogen carbonate (85.5 mg), and 2,2-dimethylmalonic acid monocyclohexyl ester (261 mg) were added, and the resulting mixture was stirred at room temperature for 3 days. Ethyl acetate (30 mL) and water (10 mL) were added to the mixture, and the resulting mixture was shaken, after which the organic layer was collected. Ethyl acetate (20 mL) was added to the aqueous layer, and the resulting mixture was shaken, after which the organic layer was collected. All the organic layers were combined, washed with saturated aqueous sodium chloride solution (10 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 heptane-ethyl acetate) to obtain the captioned compound (97.9 mg).

1. additionwere added
2. stirringthe resulting mixture was shaken
3. customafter which the organic layer was collected
4. additionEthyl acetate (20 mL) was added to the aqueous layer
5. stirringthe resulting mixture was shaken
6. customafter which the organic layer was collected
7. washwashed with saturated aqueous sodium chloride solution (10 mL)
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationThe resulting mixture was filtered
10. customthe filtrate obtained
11. concentrationwas concentrated under reduced pressure
12. customThe residue obtained
13. customwas purified by NAM silica gel column chromatography (mixed solvent of heptane-ethyl acetate)