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）， a four-step route was developed 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% with the final product purity exceeding 98%. The structures of key intermediates and products were characterized by single-crystal X-ray diffraction， nuclear magnetic resonance， and infrared spectroscopy. 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 by DSC， ARC， and RC1. The results showed that the oxidation reaction process had a high hazard level， while the nitration reaction process was classified as level 2. This synthesis route has promising potential for industrial-scale application.