Abstract: | A new process for a continuous‐flow di‐N‐alkylation of 1H‐benzimidazole to 1H‐benzimidazole‐3‐ium iodide by methylene iodide in the presence of potassium carbonate in a fixed‐bed reactor is presented. The synthesis was transferred from batch to continuous operation with similar yields and conversion rates. Moreover, the influence of temperature and residence time in the continuous flow setup was characterized; optimized conditions led to a doubling of yield. In addition, the continuous flow allowed for a better control of the two‐step reaction by adding an additional tube reactor after the fixed bed that further enhanced the overall performance. With this, the continuous‐flow system presented itself as superior due to higher available temperatures and a better controllability. |