反应详情

温度

95 °C

Process 4: Trimethylsilyl azide (8.68 g, 75.3 mmol) and dibutyltin oxide (55 mg, 0.221 mmol) were added to toluene (20 mL) solution of 2-{5-{[4-butyl-1-(5-methoxypyrimidin-2-yl)-2-methyl-6-oxo-1,6-dihydropyrimidin-5-yl]methyl}pyridin-2-yl}benzonitrile (200 mg, 0.43 mmol) and stirred for 24 hours at 95° C. under argon atmosphere. The residues obtained by removing the reaction solvent by distillation was separated and purified by silica gel column chromatography (chloroform:methanol=100:1) to give 5-{{6-[2-(1H-tetrazol-5-yl)phenyl]pyridin-3-yl}methyl}-6-butyl-3-(5-methoxypyrimidin-2-yl)-2-methylpyrimidin-4(3H)-one (174 mg, 80%) as yellow oil.

1. customThe residues obtained
2. customby removing the reaction solvent
3. distillationby distillation
4. customwas separated
5. custompurified by silica gel column chromatography (chloroform:methanol=100:1)