反应详情

To a solution of ethyl 4-bromo-3,5-dimethyl-1H-pyrrole-2-carboxylate (2.4 g, 10 mmol) in DMF (25 mL) was added tetrakis(triphenylphosphine)palladium (2.3 g, 1 mmol). After stirring 15 min, the reaction mixture was charged with 2-(trifluoromethyl)-benzeneboronic acid (2.4 g, 12.5 mmol) and sodium carbonate (in 5 mL of water). The reaction mixture was heated to reflux overnight with stirring. After cooling, the reaction mixture was then diluted with water and extracted with DCM. The combined extracts were washed with water and dried over Na2SO4. Evaporation of solvent gave a crude material, which was purified by chromatography on silica gel column eluting with EtOAc-hexane (1:1) to give the title compound (1.5 g). MS (ES): 312 (MH+)

1. temperatureThe reaction mixture was heated
2. temperatureto reflux overnight
3. stirringwith stirring
4. temperatureAfter cooling
5. extractionextracted with DCM
6. washThe combined extracts were washed with water
7. dry with materialdried over Na2SO4
8. customEvaporation of solvent
9. customgave a crude material, which
10. customwas purified by chromatography on silica gel column
11. washeluting with EtOAc-hexane (1:1)