反应详情

温度

100 °C

To a suspension of 1-{4-[4-(5-Bromo-2-morpholin-4-yl-benzoyl)-piperazin-1-yl]-3-fluoro-phenyl}-ethanone (160 mg, 0.33 mmol) in toluene (2 ml) were added PdCl2(PPh3)2 (5 mg, 0.0065 mmol) and tributyl(1-ethoxyvinyl) tin (125 ul, 0.36 mmol). The mixture was heated to 100° C. for 6 hours. The mixture was cooled in an ice bath and 2N HCl (0.55 ml) was added. The mixture was stirred at room temperature overnight. The mixture was filtered. The organic layer was separated and 10% aqueous KF solution was added. The mixture was stirred at room temperature for 3 hours and filtered. The organic layer was dried over Na2SO4, filtered and the solvent was removed in vacuo. The crude gum was chromatographed on silica gel, eluent: heptane/ethylacetate 0%-50% (10 minutes) to provide the title compound (15 mg, 10%) as a white solid MS (m/e): 454.2 (M+H, 100%).

1. temperatureThe mixture was cooled in an ice bath
2. filtrationThe mixture was filtered
3. customThe organic layer was separated
4. addition10% aqueous KF solution was added
5. stirringThe mixture was stirred at room temperature for 3 hours
6. filtrationfiltered
7. dry with materialThe organic layer was dried over Na2SO4
8. filtrationfiltered
9. customthe solvent was removed in vacuo
10. customThe crude gum was chromatographed on silica gel, eluent