Continuous synthesis of multistep polymerizations at microscale is made available by coupling two microstructured chip reactors in a single reactor setup. Conjugated [2-methoxy-5-(3,7-dimethyloctyloxy)]-1,4-phenylenevinylene (MDMO-PPV) is synthesized via the radical sulfinyl precursor route. Reactions are carried out in separate reactors and optimization of the elimination of polymer can be effectively performed in a defined temperature range, allowing for full polymer conversion within minutes and formation of conjugated materials. The combination of both processes in a single coupled reactor setup permits total monomer-to-conjugated-MDMO-PPV conversions while retaining its pristine optical properties. Polymer characteristics are comparatively good and the reduction in yield due to the lower initial monomer concentrations is compensated by the much shorter reaction times required in the flow process.