Cyclohexene dicarboxylic acid monohydrazides and sodium nitrite in the presence of acetic acid produced 2-(4-R-phenyl)-1-carboxy-4-methyl-4-cyclohexene-carbonylazides. These compounds served as starting material in the synthesis of unknown cyclohexene group containing diacylureas, when treated with derivatives of 2-aminopyridines. Reactions of 2-(4-R-phenyl)-1-carboxy-4-methyl-4-cyclohexenecarbonylazides with 2-amino-5-bromo-, 2-amino-3,5-dibromo- and 2-amino-5-methylpyridines were done in benzene or toluene in presence of catalitic amount of pyridine. In the case of benzene, N-[2-(4-R-phenyl)-1-carboxy-4-methyl-4-cyclohexene]-N’-(3-R1-5-R2-pyridyl-2)urea results, but in the case of toluene – N-[2-(4-R-phenyl)-4-methyl-4-cyclohexene]-N’-(3-R1-5-R2-pyridyl-2)urea due to formation of disubstituted urea derivatives and decarboxylation in boiling temperature of toluene.