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For the first time, micromixing characterization for the Villermaux–Dushman reaction could be performed with a non-reactive viscous medium at viscosities up to 2 Pas. As viscous medium, sucrose solution was used with the benefit of being a Newtonian fluid with tuneable viscosity. Due to the higher viscosities in comparison to established media for micromixing investigations, a new protocol for the experimental implementation was developed. Micromixing experiments were conducted and the applicability of viscous sucrose solutions was proven in a stirred tank reactor. Major challenges in characterizing micromixing efficiency in high viscous solution were consolidated.