A study was conducted to analyze the synthesis, helical organization, and fibrous formation of C 3 symmetric Methoxy-substituted discotic hexa-peri-hexabenzocoronene (HBC). HBCs were synthesized using the oxidative cyclodehydrogenations of proper hexaphenyl-benzene precursors. NMR spectroscopy was used to analyze the property of HBCs toward self-assembly in solution. The self-assembly led to fibrous nanostructures with several hundred micrometers in length upon drop-casting. Differential scanning calorimetry (DSC) was used to observe thermotropic properties of HBCs. The UV-vis and photoluminescence spectra was used to analyzed internal structure of HBCs for observing fibrous structures. Results show that HBC with three alternative dodecyl1 and methoxy substitutions was synthesized using the Scholl reaction.