Abstract 1H, 1′ H-5, 5′-Bitetrazole-1, 1′-diol was synthesized starting from glyoxal, which is converted to glyoxime after treatment with hydroxylamine. Chlorination of glyoxime with Cl 2 gas in ethanol and following chloro/azido exchange yields diazidoglyoxime, which is cyclized under acidic conditions (HCl gas in diethyl ether) to give 1H, 1′ H-5, 5′- bitetrazole-1, 1′-diol dihydrate (1). A large variety of nitrogen-rich salts of 1 such as the ...