Two approaches to the synthesis of bis-3,3'-(nitro-NNO-azoxy)difurazanyl ether 2 have been tested, that is, varying the sequence of the introduction of the nitro-NNO-azoxy group and ether bridge. Difurazanyl ether formation through base-promoted transformation of nitrofurazans has been studied in which the nitro groups were activated by ortho electron-withdrawing substituents such as nitro-NNO-azoxy and tert-butyl-NNO-azoxy groups. The nitro-NNO-azoxy group was formed by destructive N-nitration of the tert-butyl-NNO-azoxy group. The X-ray crystal structure of 2 is reported.