反应详情

Under a nitrogen atmosphere, to a mixture of ethyl 3[3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)phenyl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridine-8-carboxylate (0.28 g) in THF (5 ml) was added methylmagnesium bromide (1M THF solution, 2.61 ml) at 0° C., and the mixture was stirred at room temperature for 4 hr. The reaction mixture was diluted with ethyl acetate and saturated aqueous ammonium chloride solution, the mixture was washed with saturated brine and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane), and further recrystallized from ethyl acetate/hexane to give the title compound (0.16 g).

1. washthe mixture was washed with saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customthe solvent was evaporated under reduced pressure
4. customThe residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)
5. customfurther recrystallized from ethyl acetate/hexane