反应详情

Add methylmagnesium bromide (1.25 mL, 3.7 mmol) dropwise at 0° C. to a solution of N-methoxy-N-methyl-5-phenylethynylnicotinamide, (prepared essentially as described in PREPARATION 2), (1.0 g, 3.76 mmol). Allow the mixture to warn to room temperature overnight. Dilute with ethyl acetate and saturated ammonium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 10:90 to 30:70 tetrahydrofuran:hexanes) to give title compound as a white solid (0.70 g, 84%).

1. custom(prepared essentially
2. customas described in PREPARATION 2), (1.0 g, 3.76 mmol)
3. dry with materialdry (magnesium sulfate)
4. concentrationconcentrate
5. custompurify
6. wash(silica gel chromatography, eluting with 10:90 to 30:70 tetrahydrofuran:hexanes)