The synthesis of 1,4-dinitrofurazano[3,4-b]piperazine (DNFP) with an overall yield of 32.6%,was described. The cyclizative condensation between N,N′-di-tert-butyl ethylenediamine and dichloroglyoxime at low temperature generated 1,4-di-tert-butyl piperazine-2,3-dioxime(PDO-tB), which underwent a base-promoted dehydration at high temperature to obtain 1,4-di-tert-butylfurazano[3,4-b]piperazine (FP-tB). Furthermore, nitrolysis of FP-tB provided an efficient access to the novel explosive compound DNFP. The structures of DNFP and its intermediates were characterized by IR, ¹H NMR, ¹³C NMR and elemental analysis. Moreover, the effects of reaction conditions on the yield of PDO-tB were studied, and the optimum reaction condition is dropwise addition at -18 ℃. Converting FP-tB to DNFP with several nitrolysis reagents were also studied, and the nitrolysis with the mixed acid of 98% HNO₃ and H₂SO₄ provides a good yield of 61.7%.