反应详情

A mixture of 1-{(S)-2-[(5-Bromo-pyrimidin-2-ylamino)-methyl]-piperidin-1-yl}-1-[4-(4-fluoro-phenyl)-1-methyl-1H-pyrazol-3-yl]-methanone (0.5 g) and 1-ethoxyvinyl)tributyltin (0.42 ml) tetrakis(triphenylphosphine)palladium[0} (0.06 g) was boiled in dioxane (8 ml) for 16 h. 2N Hydrochloric acid was added, the mixture stirred for 90 min, water was added and the mixture extracted (×3) with ethyl acetate. The combined ethyl acetate extracts were dried, solvent removed at reduced pressure and the residue column chromatographed (silica gel, ethyl acetate→2% methanol ethyl acetate to give the title compound (0.3 g) as a yellow foam.

1. extractionthe mixture extracted (×3) with ethyl acetate
2. dry with materialThe combined ethyl acetate extracts were dried
3. customsolvent removed at reduced pressure
4. customthe residue column chromatographed (silica gel, ethyl acetate