反应详情

温度

130 °C

A resealable reaction tube was charged with cesium carbonate (0.873 g, 0.268 mmol), 3-bromo-4-chloropyridine hydrochloride (0.205 g, 0.894 mmol) and 4-(4-phenylphthalazin-1-ylamino)phenol (0.280 g, 0.894 mmol) and purged with nitrogen for several minutes. 1.8 mL of DMSO was added, the tube was sealed, and the reaction mixture was heated to 130° C. for 3 h. Upon cooling the mixture was diluted with EtOAc and washed with water. The aqueous portion was extracted with EtOAc, and the combined organic portions were dried with MgSO4 and concentrated. N-(4-(3-bromopyridin-4-yloxy)phenyl)-4-phenylphthalazin-1-amine was isolated as an orange solid. MS m/z=470 [M+H]+. Calc'd for C25H17BrN4O: 469.33.

1. custompurged with nitrogen for several minutes
2. addition1.8 mL of DMSO was added
3. customthe tube was sealed
4. temperatureUpon cooling the mixture
5. additionwas diluted with EtOAc
6. washwashed with water
7. extractionThe aqueous portion was extracted with EtOAc
8. dry with materialthe combined organic portions were dried with MgSO4
9. concentrationconcentrated