3,4-Diaminofurazan

2580-79-2

17220-38-1

The general procedure for the synthesis of 3,4-diaminofurazan from diaminoglyoxime is as follows: Example 1: Synthesis of 3,4-diaminofurazan. In a 500 mL round-bottomed flask equipped with a mechanical stirrer and a thermometer, ethylene glycol (150 mL) was heated to 120 °C. To this hot solution, diaminoglyoxime (50 g, 0.42 mol) and potassium hydroxide (24 g, 0.42 mol) were added sequentially. The reaction mixture was warmed to 170 °C and maintained at this temperature for 1 hour. Upon completion of the reaction, the clarified reaction solution was cooled to room temperature and subsequently slowly poured into a mixture consisting of ice (500 g) and water (100 mL). The mixture was stirred vigorously for 5 minutes until 3,4-diaminofurazan precipitated as solid crystals. The precipitate was collected by filtration, washed with cold water (20 mL) and subsequently dried in air overnight to give 22 g of an off-white solid product (52% yield) with a melting point of 179-181 °C (literature value: Gunasekaran, A. et al., 179-180 °C). The 1H NMR (DMSO-d6) data of the product were as follows: δ 5.81 (s) ppm.