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Reported herein is a multidisciplinary laboratory experiment for advanced undergraduate students that includes elements of material synthesis, in the synthesis of cyclodextrin-containing metal–organic frameworks (CD-MOFs), and environmental chemistry, in the use of these MOFs for pollutant removal. This multiday laboratory experiment starts with the synthesis of cyclodextrin-containing metal–organic frameworks (CD-MOFs) using vapor diffusion crystal growth procedures, followed by the use of the CD-MOFs for a pollutant removal application. Specifically, the CD-MOFs were used for the removal of a methylene blue dye (a common mimic of aromatic pollutants) from an organic solution, with the monitoring of the success of the removal procedures using UV–vis spectroscopy. This experiment was implemented as part of a larger multiday unit, and undergraduate students were particularly engaged with and excited by the CD-MOF synthesis and methylene blue removal experimental modules. As a result, the decision was made to make these two components a stand-alone multidisciplinary laboratory experiment, the results of which are reported herein.