The synthesis of end-capped thieno[3,2-f:4,5-f′]bis[1]benzothiophene was achieved from thiophene and 2,5-thiophenedicarboxaldehyde. Specifically, hexyl and dodecyl end-capping groups conferred reversible redox behavior as evidenced by cyclic voltammetry with oxidation potentials of 0.73V versus Fc/Fc+ couple. An extensive spectrophotometric analysis is reported.