17645-17-9

823-58-5

74-89-5

17645-17-9

General procedure: in an autoclave, 3,6-dichloropyridazin-4-amine (2.35 g, 14.3 mmol) was dissolved in ethanol (20.2 g, 215 mmol, 26.7 mL), methylamine was added and the mixture was heated to 100 °C. The reaction was continued at 100 °C for 48 h until LCMS analysis showed complete consumption of the feedstock. Subsequently, the reaction mixture was evaporated to dryness. The crude product was dissolved in dichloromethane, triethylamine (4 mL) was added and the solvent was evaporated after stirring for 5 minutes at room temperature. The residue was diluted with water (5 mL) and the insoluble material was collected by filtration and dried to give 6-chloro-N3-methyl-3,4-pyridazinediamine (1.35 g, 57% yield) as a light brown solid.LCMS (method ZCQ13) analysis showed a retention time of 0.17 min and a mass-to-charge ratio of 157/159 (M-H).