Two different concepts for the modularization and automation of microreaction systems are described. The modular microreaction system FAMOS was developed on the basis of a functional toolkit concept for laboratory applications of microreaction technology. Microstructured reaction modules with suitable fluidic, analytical and electronic interfaces were designed which allow the realization of even multi-stage microchemical processes like the sulfonation of toluene under thermally controlled conditions over the entire process. The automated microreaction system AuM mu Res was developed to enable an active regulation of process parameters via a process control system to perform parameter screenings for the identification of process optima. Integrated microstructured flow-through sensors and analytical interfaces were developed for the monitoring of relevant process parameters. Sampling devices for chromatographic analysis and inline Raman spectroscopy were integrated into the micoreaction system to gather relevant analytical information about the considered chemical process. By applying chemometric models, a qualitative and quantitative realtime monitoring of microchemical processes was established, as was demonstrated for different nitration reactions.