Recent advances in benchtop NMR has facilitated a non-invasive method for real-time monitoring, characterization, and quantification of chemical entities, becoming a practical analytical tool for precise reaction monitoring, condition optimization, and quantitative information on purity and yield directly in the laboratory. Past studies utilize benchtop spectrometers as a low-cost and user-friendly alternative to high-field spectrometers for the heteronuclear characterization of various materials including lignins , fluorinated environmental contaminants , peptide structure , drug identification , and many others. Proton lock capabilities on benchtop spectrometers have allowed heteronuclear NMR-based reaction monitoring without requiring the use of deuterated solvents, which can be financially prohibitive for reactions performed on scale. Furthermore, spectra can be acquired in mere seconds directly in a synthetic laboratory, allowing for rapid and real-time quantification of chemical entities in a crude reaction mixture without further processing or sample preparation . Here, we implement benchtop F NMR to screen reaction conditions in the conversion of 5-FU into carmofur.