Abstract: The acetylation of 3,4-diaminofurazan, the nitration of its acetylated products and the rearrangement-decomposition of nitrated products were studied in this work. Under the catalysts of p-Toluenesulfonic acid, the products of 3-amino-4-acetylaminofurazan and 3, 4-diacetyl-aminofurazan were got respectively by using acetic acid and acetic anhydride to acetylate 3,4-diaminofurazan. It is found that, when the reaction time is 3 hours for 3-amino-4-acetylaminof-urazan and 10 minutes for 3,4-diacetyl-aminofurazan, the yields of products reach the maximum of 78% and 89%, respectively. The 3-acetylamino-4-nitrylaminofurazan was also prepared when 3,4-diacetylaminofurazan was nitrified in the mixture of nitric acid and acetic anhydride and the maximum yield is 54% when the reaction temperature between 0℃ and -5℃. Under the catalysts of dram acid, the rearrangement and following with decomposition reaction of 3-acetylamino-4-nitryl-aminofurazan surrounded in THF would occur to yield 3-acetylaminofurazan.