反应详情

温度

90 °C

5-Bromo-N-(2-cyclopropyl-2-hydroxy-propyl)-6-(2,2,2-trifluoro-ethoxy)-2-trifluoromethyl-nicotinamide (0.09 g, 0.19 mmol) was dissolved in toluene (4 mL) and dimethylformamide (0.3 mL). To this solution was added with stirring [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) CH2Cl2 (8 mg, 0.010 mmol), 4-chlorophenylboronic acid (32 mg, 0.20 mmol) and sodium carbonate solution (2M, 0.20 mL). This mixture was heated to 90° C. for 15 h and cooled to room temperature. Water (10 mL) was added, the phases were separated and the water mixture was extracted with ethylacetate. Organic phases were pooled, dried with MgSO4 and the volatiles removed in vacuo. The residue was purified by flash chromatography (SiO2, dichloromethane/ethyl acetate) to give the title compound (53 mg) as a brown gum; MS (ISP) 497.2 (M)+.

1. temperaturecooled to room temperature
2. customthe phases were separated
3. extractionthe water mixture was extracted with ethylacetate
4. dry with materialdried with MgSO4
5. customthe volatiles removed in vacuo
6. customThe residue was purified by flash chromatography (SiO2, dichloromethane/ethyl acetate)