<p>The separation of 2,2-dimethoxypropane (DMP) from reaction masses is an important process in chemical manufacturing, particularly in the combination of fine chemicals and pharmaceuticals. This review critically evaluates various separation techniques employed to isolate DMP from complex reaction mixtures. It encompasses a comprehensive analysis of traditional approaches such as concentration and liquid–liquid extraction, highlighting their efficiency, limitations, and suitability based on the physical and chemical properties of DMP. The review also addresses the integration of novel technologies, such as membrane separation and advanced adsorption materials, which offer promising solutions to existing challenges in separation efficiency and cost. Comparative analysis of these methods reveals trends towards more sustainable and cost-effective approaches, with a focus on reducing environmental impact and improving process scalability. Special emphasis is placed on recent innovations and improvements in separation methods, such as the use of novel adsorbents and catalysts, which contribute to higher purity and yield of DMP. The review addresses challenges associated with the separation process, including the impact of impurities, reaction conditions, and economic considerations. Comparative performance metrics and case studies from recent literature are discussed to provide insights into the practical application of these techniques. The review aims to offer a detailed understanding of the current state of DMP separation technologies, guiding researchers and industrial practitioners in selecting and optimizing appropriate methods for their specific needs.</p>