反应详情

温度

90 °C

To a suspension of 4-(3-bromo-5-chlorophenoxy)-5-chloro-1H-indazole (40 g, 112 mmol) and zinc cyanide (15.74 g, 134 mmol) in DMF (400 mL) was added palladium tetrakis triphenylphosphine (38.7 g, 33.5 mmol) and heated to 90° C. for 1 hour. After this time, the reaction was cooled to room temperature and partitioned between saturated aq. NH4Cl (500 mL), water (500 mL) and EtOAc (2×1000 mL). The combined extracts were dried over MgSO4, absorbed onto silica gel (200 g) and the solvent removed in vacuo. This solid was purified on a silica gel (1000 g) column (0-10% EtOAc/CH2Cl2) to give the title compound as a white solid. LRMS (M+1)=303.9

1. temperatureAfter this time, the reaction was cooled to room temperature
2. custompartitioned between saturated aq. NH4Cl (500 mL), water (500 mL) and EtOAc (2×1000 mL)
3. dry with materialThe combined extracts were dried over MgSO4
4. customabsorbed onto silica gel (200 g)
5. customthe solvent removed in vacuo
6. customThis solid was purified on a silica gel (1000 g) column (0-10% EtOAc/CH2Cl2)