This study presents synthesis of novel block copolymers of thienyl end capped polysulfone and polypyrrole via chemical oxidative polymerization by iron (III) chloride. Polysulfone is synthesized from bisphenol and bis (p-chlorophenyl) sulfone in presence of potassium carbonate. Polysulfone (PSU) was reacted with 2-thiophenecarbonyl chloride in order to synthesize a macromonomer containing thienyl end-group (PSU-ThC). Then copolymers of PSU-ThC and pyrrole were synthesized by chemical oxidative polymerization using iron (III) chloride as an oxidant. The synthesized block copolymers (PSU-ThC-b-PPy) were characterized by spectroscopic analysis and the electrical conductivities were investigated with 4-point probe technique. The obtained samples were also characterized morphologically by Scanning Electron Microscope (SEM).