A novel energetic intermediate 3-amino-4-hydroxyaminoximinofurazan (DOAF) was synthesized from 3-amino-4amidoximinofurazan (DAOF) via diazotisation and oximation reactions with a total yield of 61.8%, and its structure was characterized by NMR, IR, MS and elemental analysis. The main factors for the oximation reaction were thoroughly studied, and the optimum reaction conditions were found to be as follows: the materials ratio n(ACOF)∶n(NH 2 OH•HCl)∶n(CH 3 ONa) was 1∶2∶3, reaction temperature 30 ℃, and reaction time 2 h with a yield of 86.5%. It was found that 3-amino-4-hydroxyaminoximinofurazan (DOAF) was disproportionated to obtain two compounds under alkaline condition, which were identified as 3-amino-4-nitrosoximinofurazan potassium salt and DAOF. Moreover, DOAF was hydrolyzed to give a new product in acidic aqueous solution, which was identified as 3-amino-4-(N-hydroxyamido)furazan. The single crystal of K(DNOF)•H 2 O was obtained and its crystal belong to monoclinic system, space group is P2(1)/c, cell parameters are a＝ 0.7639(19) nm, b＝0.7034(17) nm, c＝1.436(4) nm, α＝90°, β＝101.025(3)°, γ＝90°, V＝0.7573(3) nm 3 , Z＝4, D c ＝1.870 g•cm -3 , μ＝0.695 mm -1 , F(000)＝432, R 1 ＝0.0349 and wR 2 ＝0.1027.

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A novel synthetic route of [1,2,5]oxadiazolo[3,4-e][1,2,3,4]tetrazine 4,6-diN oxide (FTDO) was designed and FTDO was synthesized from 3,4-diaminofurazan (DAF) via the reactions of oxidation, condensation, nitration and cyclization with a total yield of 30.89%. FTDO and its intermediates were characterized by NMR, IR, MS and elemental analysis etc. The mechanism of cyclization was proposed and the conditions for the reaction of nitration and cyclization were optimized. It was found that the optimal conditions for the reaction of nitration were followed as: nitration reagent was 100% HNO 3 , the reaction temperature was at 25 for 2 ℃ h with a yield of 99.54%. The optimal conditions for the reaction of cyclization were followed as: the reaction temperature was at 55 , the m ℃ olar ratio of compound 4 and P 2 O 5 was 1∶16, and the volume of solvent was 160 mL/g with a yield of 46.37%.