The implementation of process analytical technologies is rapidly growing in the chemical industry as data-rich experimentation becomes more relevant. Such tools are often incorporated into flow reactors, where data collection is particularly relevant in process research. A laboratory project devised for third-year undergraduate chemistry students that combines continuous flow chemistry with inline nuclear magnetic resonance (NMR) monitoring was developed and evaluated. The student project provides hands-on experience in basic flow chemistry tools and process monitoring strategies via the generation of real-time reaction data using a benchtop NMR spectrometer in flow mode. The project also includes a second synthetic step in batch mode and structure elucidation using 1D and 2D NMR spectroscopy.