反应详情

To a mixture of 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}benzamidine acetic acid salt [CAS No. 951803-91-1] (5.6 g) and DMF (200 mL), benzoic acid 4-nitrophenyl ester (2.89 g) and triethylamine (4.7 mL) were added, and the resulting mixture was stirred overnight at room temperature. Acetic acid (6.5 mL) was added to the reaction solution, and then the solvent was evaporated under reduced pressure. The residue obtained was crudely purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid), and the crudely purified product obtained was purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (4.48 g).

1. customthe solvent was evaporated under reduced pressure
2. customThe residue obtained
3. customwas crudely purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid)
4. customthe crudely purified product obtained
5. customwas purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate)