反应详情

To a solution of 4-(8-(3,4-difluorophenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-ylamino)-1-(6-methylpyrimidin-4-yl)piperidine-4-carbonitrile (Example 231) (50 mg, 112 μmol) in THF (2 mL) was added methylmagnesium bromide (1.4 M in toluene:THF, 240 μL, 336 μmol) dropwise at 0° C., and the resulting mixture was allowed to warm up to room temperature and stirred for 3 hours. Then the mixture was quenched with saturated aqueous ammonium chloride solution and extracted with ethyl acetate. The organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated. Purification by chromatography (silica gel, 10 g, 0 to 10% methanol in dichloromethane) afforded the title compound (9 mg, 19%) as a light yellow solid.

1. customThen the mixture was quenched with saturated aqueous ammonium chloride solution
2. extractionextracted with ethyl acetate
3. washThe organic layers were washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customevaporated
7. customPurification by chromatography (silica gel, 10 g, 0 to 10% methanol in dichloromethane)