The synthesis of the novel macrocycle rings derived from bola-shaped diester–dicarboxylic acid in addition to syntheses of macro cyclic tetra lactones with various diacids and ditosylated diols ring compounds. The structures of these compounds are established by electro spray ionization mass spectrometry (ESI-MS), Fourier transform infrared spectroscopy (FT-IR), FE-SEM, NMR spectroscopic methods and thermal decomposition experiments using Mettler Toledo TGA/DSC1, STARe under a nitrogen atmosphere. The heating rate of the thermal decomposition employed was 10°C min-1, wherever applicable.