反应详情

温度

0 °C

To a solution of 7-(4-chlorophenyl)-2-((2-(hydroxymethyl)-6-(trifluoromethyl)pyridin-3-yl)methyl)-8-(pyridin-4-yl)-[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one (26 mg, 0.05 mmol) in anhydrous DMF (0.5 mL) cooled at 0° C. was added sodium hydride (60% in oil, 4.0 mg, 0.1 mmol). The resulting mixture was stirred at 0° C. for 30 min, then iodomethane (20 μL, 0.25 mmol) was added. The reaction mixture was stirred at 0° C. for 30 min, then quenched by addition of water. The mixture was extracted with EtOAc (10 mL×2), and the combined EtOAc extracts were washed with saturated aqueous NaCl, dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified using a silica gel cartridge (4 g) eluted with a gradient of ethyl acetate (50-100%) in hexanes to afford 12 mg of the title compound as a yellow foam. HPLC/MS: retention time=2.93 min, [M+H]+=526.1.

1. stirringThe reaction mixture was stirred at 0° C. for 30 min
2. customquenched by addition of water
3. extractionThe mixture was extracted with EtOAc (10 mL×2)
4. washthe combined EtOAc extracts were washed with saturated aqueous NaCl
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified
8. washeluted with a gradient of ethyl acetate (50-100%) in hexanes