反应详情

温度

80 °C

A mixture of Example 369D (1.700 g, 2.93 mmol), 5-bromo-N-methylpicolinamide (0.757 g, 3.52 mmol), 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride dichloromethane complex (0.096 g, 0.117 mmol), and saturated sodium bicarbonate solution (10 mL, 2.93 mmol) in N,N-dimethylformamide (40 mL) was degassed and heated at 80° C. for 2 hours. The reaction mixture was filtered, treated with water and brine and extracted twice with ethyl acetate. The combined organic layers were washed with water, dried over MgSO4, filtered, concentrated, and purified on an 80 g silica column using the ISCO Companion flash system eluting with heptanes/ethyl acetate (3:7 to 2:8) to give the title compound. MS (ESI+) m/z 588.1 (M+H)+.

1. filtrationThe reaction mixture was filtered
2. additiontreated with water and brine
3. extractionextracted twice with ethyl acetate
4. washThe combined organic layers were washed with water
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified on an 80 g silica column
9. washeluting with heptanes/ethyl acetate (3:7 to 2:8)