反应详情

A mixture of 4-chloro-5-phenyl-1H-pyrazolo[3,4-c]pyridazine (155 mg, 0.67 mmol), bromine (51 μL, 1 mmol) and triethylamine (98 μL, 0.7 mmol) in chloroform (4 mL) was stirred at room temperature for 1 h. Additional bromine (25 μL) and chloroform (4 mL) were added and the reaction mixture was stirred at room temperature for 4 h. Further bromine (25 μL) and triethylamine (98 μL) were added and the reaction mixture was stirred at room temperature for 16 h. The reaction mixture was diluted with CH2Cl2 and a sodium bicarbonate solution. The aqueous phase was extracted with CH2Cl2 and the combined organic phases were dried (phase separator cartridge) and concentrated in vacuo. The resultant residue was purified using chromatography (silica gel, ethyl acetate/isohexane 0:1 to 1:1), to provide Compound Ibb as a solid (97 mg).

1. stirringthe reaction mixture was stirred at room temperature for 4 h
2. stirringthe reaction mixture was stirred at room temperature for 16 h
3. extractionThe aqueous phase was extracted with CH2Cl2
4. customthe combined organic phases were dried (phase separator cartridge)
5. concentrationconcentrated in vacuo
6. customThe resultant residue was purified