3-(4-Iodophenoxy)-tris(2-nitrobenzenesulfonyl)-1,4,7-triazacyclodecane (5a ) was synthesized by a Mitsunobu reaction between pernosylated diethylenetriamine (4a ) and 1,3-bis(trityloxy)propan-2-ol(2). 5a served as a key intermediate in the preparation of MRI contrast agents allowing biomolecule labeling both in solution and on solid phase.