Synthesis of Diaminoglyoxime from Glyoxal

In a beaker 140 g of sodium hydroxide is dissolved in 220 mL of ice and the solution is cooled down to 0°C, then 222 g of hydroxylamine hydrochloride is added to the solution with stirring, 116 g of 40% glyoxal solution is added to the solution with stirring and the solution is placed into a freezer for 10 minutes. The solution is heated at 90-100°C for 5h with condenser trap, cooled down in a freezer, filtered and poured into 400 mL of hot water. The diaminoglyoxime slowly recrystallized from the water. (Using microwave for 3 minutes instead of the heating at 5h will give you 20% more product)



Heating the solution at 90-100°C for 5h with the condenser trap


The diaminoglyoxime precipitated in the freezer


The recrystallization of the precipitated product

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