In this work we set out to monitor the synthesis of two quinoxalines. Quinoxalines are important in the pharmaceutical industry. Their anticancer, antiviral, and antibacterial properties have been explored with promising results for therapeutic uses. The synthesis of quinoxalines via solvent free, or low solvent routes is of great interests as many pharmaceuticals containing quinoxalines are sold as solids, and have low solubility. Using mechanochemical methods provides a direct, solvent free route to these compounds while introducing green, safe, and efficient process into the pharmaceutical industry, process that are in high demand. In addition to the advantages to mechanochemical synthesis, the industry will greatly benefit from time domain solid-state MR measurements that are reported in this work. The methods used contain no workup, particularly for in-process analysis/checks are required, leading to better optimization of reactions. Previous work from our group outlines the use of polytetrafluoroethylene (PTFE) milling jars such that both synthesis and T1-T2* measurements can be done in without the isolation of the product, providing further in situ monitoring. The combination of our T1-T2* correlation measurement, mechanochemical processes, and magnetic resonance measurements are promising for both academic, but industrial applications.