反应详情

2-Bromo-N-[4-methoxy-3-(4-methyl- 1-piperazinyl)phenyl]-3-methoxythiophene-4-carboxamide (0.20 g;0.45 mmol) was stirred with 4-pyridylboronic acid (0.056 g;0.45 mmol), tetrakis(triphenylphosphine)palladium(0) (0.024 g) and anhydrous sodium carbonate (0.053 g;0.50 mmol) in water (5 ml) and DME (5 ml) and the whole heated at reflux under Ar (18 hours). The reaction mixture was poured into 10% Na2CO3 (aq) (20 ml) and extracted into CHCl3. The organic extracts were combined, dried over Na2SO4, filtered and the filtrate evaporated in vacuo to a brown gum. The gum was purified by flash silica-gel chromatography and eluted with 4%MeOH/CHCl3 to yield a orange gum (0.088;44%).

1. temperaturethe whole heated
2. temperatureat reflux under Ar (18 hours)
3. extractionextracted into CHCl3
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customthe filtrate evaporated in vacuo to a brown gum
7. customThe gum was purified by flash silica-gel chromatography
8. washeluted with 4%MeOH/CHCl3
9. customto yield a orange gum (0.088;44%)