In this presentation, we will describe our approach for developing continuous processes, and present the application of this approach to an oxidative nitration reaction of a nitroalkane. We carried the product of oxidative nitration forward and reacted it with formaldehyde to form the corresponding 2,2-dinitroethanol derivative and isolated the product by means of a continuous pH adjustment. We will describe the advantages of performing data-rich experiments using automated lab reactors, collecting reaction calorimetry data, and using in situ Raman spectroscopy for this type of project, and present the results of a lab-scale demonstration of the continuous process with on-line Raman monitoring used as an in-process control to ensure acceptable product quality.