To improve the safety and reduce the toxicity of the synthesis process for 3,4-bis(4-nitro-1,2,5-oxadiazol-3-yl)-1,2,5-oxadiazole-2-oxide (DNTF), DNTF was synthesized via a four-step sequence starting from 1,3-acetonedicarboxylic acid, involving oximation, cyclization, oxidation, and nitration. The synthesis employed two critical intermediates: 3-amino-4-(carboxymethyl)furazan (formed after cyclization) and 3-nitro-4-(carboxymethyl)furazan (generated during nitration). The process achieved an overall yield of 22% while maintaining a purity exceeding 98% for the final product. The structures of key intermediates and products were characterized by single-crystal X-ray diffraction, nuclear magnetic resonance, infrared spectroscopy, and other techniques. The optimal synthesis process was determined through single factor experiments, with an oxidation reaction yield of 97% and a nitration reaction yield of 56.5%. The process safety risks of oxidation and nitration reactions were studied through DSC, ARC, and RC1. The results showed that the oxidation reaction process had a high degree of danger, while the nitration reaction process had a level 2 danger. This process has certain engineering prospects.