反应详情

Methylmagnesium bromide (0.199 mL of 3M solution, 0.28 mmol) was added slowly to a solution of 1-(2-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenylamino)-5-methyl-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-yl)ethanone (25 mg, 0.06 mmol) in THF (3 mL). The mixture was stirred at RT for 1 h. The mixture was quenched with saturated solution of ammonium chloride in water (1.5 mL) and diluted with brine (10 mL). The mixture was extracted with EtOAc (2×20 mL). The organic phase was dried over sodium sulfate and concentrated in vacuum. The residue was purified by preparative HPLC to give title compound as a dry film, 13 mg (45%).

1. customThe mixture was quenched with saturated solution of ammonium chloride in water (1.5 mL)
2. additiondiluted with brine (10 mL)
3. extractionThe mixture was extracted with EtOAc (2×20 mL)
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated in vacuum
6. customThe residue was purified by preparative HPLC