An AB 2 monomer PhBr 2 ACBCAPhACBCH containing one acetylene group and two bromide groups was efficiently synthesized by a strategy based on the different reactivity between aromatic iodide and bromide in Sonogashira reaction. The Sonogashira polymerization of PhBr 2 ACBCAPhACBCH was investigated to get hyperbranched poly(p-phenyleneethynylene-alt-mphenyleneethynylene) (hb-PMPE) in terms of the effects of monomer addition method, core molecule with different functionality, and ratio of INTRODUCTION Because of the highly branched and globular structure, hyperbranched conjugated polymers exhibit better solubility, thermal stability, and processibility than their linear analogues; therefore, it is much easier for them to form amorphous films of high quality and morphological stability. Moreover, the hyperbranched structure can enhance exciton confinement, suppress intrachain and interchain exciton annihilation, thereby, improve fluorescence quantum yields and electroluminescent efficiency significantly. 1 The global molecular shape can also induce efficient intramolecular energy transfer. [2][3][4] Hyperbranched conjugated polymers have attracted considerable attention as novel materials in the fields of light emitting, 5-23 solar cells, 24-26 fluorescent chemosensors, 27-32 and so on.