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In this work, for a series of 1-(5-nitro-1,3-dioxan-5-yl)-1H-1,2,3-triazole derivatives, we studied the possibility of nitro group transformation by the action of triethyl phosphite. It was found that 1,3-dioxane cycle expands to 4,7-dihydro-1,3,5-dioxazepines when heated in benzene with an excess of reducing agent.