In this laboratory experiment, the synthesis and characterization of H[subscript 5]PV[subscript 2]Mo[subscript 10]O[subscript 40]@Cu[subscript 3](BTC)[subscript 2] (denoted as NENU[subscript -9], H[subscript 3]BTC = 1,3,5-benzenetricarboxylic acid) and its application in fuel desulfurization were performed. This experiment is designed for advanced undergraduate students majoring in chemistry. In this experiment, students experience the universal procedures of solution syntheses, get knowledge of several modern instrumental techniques (PXRD, FTIR, SEM, and GC) widely utilized in chemical research, and learn the general procedure of heterogeneous catalytic reaction. Upon the completion of the experiment, not only was students' teamwork spirit cultivated by data-sharing and discussion in their assigned group, but also their environmental protection awareness was stimulated by performing a catalytic oxidative desulfurization reaction, a potential technology that may reach the goal of reducing sulfur oxide emissions. Moreover, students' basic chemistry knowledge (inorganic, coordination, organic, and analytical chemistry) was consolidated by using it to analyze experimental phenomena and results.