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Hydroformylation represents an important homogeneous catalyzed process, which is widely used within chemical industry. Usually applied for short-chained alkenes like Propene and Butene aldehydes obtained from alkenes >C6 are relevant intermediates in production of plasticizers, surfactants and polymers. Today the active catalyst species is often based on valuable Rhodium complexes in aqueous solution. This implies the problem of limited water solubility of the reactants, which is acceptable for short chain lengths, but states a problem in case of higher alkenes. Along with that efficient separation and recycling of the catalyst becomes more complicated. There are different approaches tackling this problem, e.g., by using of salt formation in the BASF process or downstream distillation within the Shell process. Another promising approach is the processing within a microemulsion by using a suitable surfactant system. This maintains a large interface between catalyst and reactants, as well as the possibility of catalyst recycling via downstream phase separation in a settler. Optimized processing within the three-phase region in accordance with Kahlweit fish leads to an efficient product separation, while the valuable catalyst and surfactant can be recycled into the process. In this work we present reaction monitoring of Rh-catalyzed hydroformylation of 1 dodecene. Experiments were conducted on a specialized laboratory setup, which allows coupling of different online spectroscopic methods (Raman, HR-NMR, LF-NMR, UV/VIS) under process-similar conditions. The focus of this contribution lies on results of high-resolution Online-NMR obtained during calibration experiments for development of a multivariate model for Raman spectroscopy, which will be part of another contribution.