反应详情

1-(2-(3-Methoxy-4-(4-methoxy-1H-imidazol-1-yl)phenylamino)-6-((2,2,2-trifluoroethoxy)-methyl)pyrimidin-4-yl)ethanone (145 mg, 0.32 mmol) was coevaporated with dioxane and dissolved in THF (10 mL). The mixture was added slowly to a well stirred solution of methylmagnesium bromide (0.857 mL, 3 M solution, 2.57 mmol) in THF (5 mL). The mixture was stirred at rt for 5 min. The mixture was cooled on ice bath and ammonium chloride (aq, 5 mL) was added. The mixture was extracted with ethyl acetate (2×10 mL), the organic phase was filtered and concentrated in vacuum. The residue was separated purified by preparative HPLC to give the title compound as a dry film, 68 mg (46%).

1. additionThe mixture was added slowly to a well
2. temperatureThe mixture was cooled on ice bath
3. extractionThe mixture was extracted with ethyl acetate (2×10 mL)
4. filtrationthe organic phase was filtered
5. concentrationconcentrated in vacuum
6. customThe residue was separated
7. custompurified by preparative HPLC