反应详情

Add a 3.0 M solution of methylmagnesium bromide (1.25 mL, 3.8 mmol) in diethyl ether dropwise to a cooled solution of N-methoxy-N-methyl-5-phenylethynyl -nicotinamide, (prepared as described in PREPARATION 2), (1.00 g, 3.7 mmol) in tetrahydrofuran (8.0 mL) at 0° C. Warm to room temperature, stir overnight and dilute with ethyl acetate. Wash with an aqueous saturated solution of ammonium chloride, dry (magnesium chloride), filter and concentrate. Purify the residue by silica gel chromatography, eluting with 10:90 to 30:70 tetrahydrofuran:hexanes, to give the title compound as a white solid (0.70 g, 84%).

1. washWash with an aqueous saturated solution of ammonium chloride
2. dry with materialdry (magnesium chloride)
3. filtrationfilter
4. concentrationconcentrate
5. customPurify the residue by silica gel chromatography
6. washeluting with 10:90 to 30:70 tetrahydrofuran