In a beaker solution is made from 27.5 g of very cold 50% hydrogen peroxide, 17.5 of ice and 30 g of ammonium persulfate, to this solution slowly, with very vigorous stirring to create foam, a solution made from 2.5 g of 3,3′-diamino-4,4′-azoxyfurazan and 32 g of conc. sulfuric acid is added. The temperature should be maintained below 20°C. The solution is then heated at 40°C and stirred vigorously for 9h, then the solution is poured into 200 mL of water and the product is extracted with 150 mL of DCM, the DCM layer is washed with some dilute sodium bicarbonate solution and then evaporated to dryness. The pure product may be recrystallized from warm DCM.
The reaction taking place and crystals of the product