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The key synthetic stage (cyclization) of 9-(2-diethylaminoethyl)-2-phenylimidazo[1,2-α]benzimidazole dinitrate, which possesses antiulcer activity, was improved by changing the reaction medium and using the imine itself rather than its hydrobromide for the cyclization. A method using the physicochemical properties (NMR and IR spectroscopy and UV spectrophotometry) of the substance was proposed for identifying it. An HPLC method was proposed for determining related impurities; nonaqueous titration, for quantitative determination. Acute toxicity was studied in mice and rats upon intragastric and intravenous administration. The results showed that the drug substance had class 3 moderate toxicity upon both intragastric and intravenous administration.