preparation method | to 3,6-dichloro-4-carboxyl-pyridazine (7.5g,38.9mmol, aldrich) of DCM(30mL) and MeOH(10mL) solutions are slowly added (trimethylsilyl) diazomethane (2.0M hexane solution) through a syringe until continuous yellow color is observed. After the addition is complete, the solvent is removed by vacuum. The crude product was purified by SiO2 chromatography and eluted with EtOAc/hexane gradient (10 to 25% EtOAc) to give 3.89g(86%) of brown oily methyl 3, 6-dichloropyridazine-4-formate, which solidified when standing. |