[摘要]:New substituted thieno[3,4-c]cinnoline-3-carboxylates were synthesized from the corresponding 3-aminothiophene-2-carboxylates by a new route using a modified Sandmeyer reaction. Under proper conditions, Sandmeyer reaction led to the formation of thieno[3,4-c]cinnolines by a regioselective intramol. cyclization, instead of the expected substitution of the NH2 group by a Br atom.