反应详情

Under nitrogen atmosphere, triethylamine (0.348 mL) was added under ice-cooling to a mixture of 4-pyridinecarboxylic acid [CAS No. 55-22-1] (61.6 mg), TFFH (132 mg), and dichloromethane (5 mL), and the resulting mixture was stirred for 1 hour. To the mixture, a mixture of N-[1-amino-1-(4-{[[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 1a, 150 mg), DMAP (5 mg), and DMF (2.5 mL) was added dropwise. After stirring the resulting mixture at room temperature for 3 days, the solvent in the mixture was concentrated under reduced pressure. The residue obtained was purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid) to obtain the captioned compound (188 mg).

1. additionwas added dropwise
2. concentrationthe solvent in the mixture was concentrated under reduced pressure
3. customThe residue obtained
4. customwas purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid)