The synthesis of 1,1-diamino-2,2-dinitroethene (FOX-7) by nitration of 4,6-dihydroxy-2-methylpyrimidine and hydrolysis of the resulting intermediate 2-dinitromethylene-5,5-dinitropyrimidine-4,6-dione has been studied. By varying the reaction parameters the optimal conditions for the synthesis of FOX-7 have been identified and gave a >90% yield of the pure product. The optimised process allowed the spent acid to be recycled without loss of yield, with almost stoichiometric consumption of nitric acid. The purity of the FOX-7 has been determined using a newly developed HPLC method
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