反应详情

3-Amino-2-4-dichloropyridine d (0.7047 g, 4.32 mmol), phenylboronic acid (0.5177 g, 4.24 mmol), K2CO3 (0.8023 g, 5.80 mmol), and Pd(PPh3)4 (0.0702 g, 0.0607 mmol) were combined. The sample was evacuated and purged with nitrogen three times. Dry DMF (2 mL) and deoxygenated H2O (0.4 mL) were added. The sample was microwaved at 130° C. for 40 minutes. The reaction mixture was diluted with H2O (50 mL) and extracted with EtOAc (3×50 mL). The EtOAc extracts was dried over MgSO4 and filtered. The crude material was adsorbed onto silica gel and purified by flash chromatography (40 g SiO2, 0-30% EtOAc in hexanes) to give 3-amino-4-chloro-2-phenylpyridine e (0.435 g, 2.12 mmol, 49%).

1. customThe sample was evacuated
2. custompurged with nitrogen three times
3. customDry DMF (2 mL) and deoxygenated H2O (0.4 mL)
4. additionwere added
5. customThe sample was microwaved at 130° C. for 40 minutes
6. additionThe reaction mixture was diluted with H2O (50 mL)
7. extractionextracted with EtOAc (3×50 mL)
8. dry with materialThe EtOAc extracts was dried over MgSO4
9. filtrationfiltered
10. custompurified by flash chromatography (40 g SiO2, 0-30% EtOAc in hexanes)