Cleavage of alkoxy-ethers in the presence of molten pyridinium chloride at high temperatures resulted in the fully ring-closed triangulenium core 3.PF6 along with complementary bocdeprotection. The second amine insertion at the oxa-bridge was done with 1-(3-aminopropoxy)-2methoxyethane at a refluxing temperature of acetonitrile but the reaction was comparatively slower with slightly smaller yields than the first amine insertion. By using a tosyl-protected-PEG derivative, two PEG-3 chains attached at the free primary amine of 4.PF6. The presence of potassium carbonate and potassium iodide promoted the efficient removal of the tosyl group to improve the overall yield of the desired product 5.PF6. Following a previously reported anion exchange procedure, the hexafluorophospahte was exchanged by chloride ion to obtain the final product (Nuc-DAOTA + ).