A microscale isotopic labeling experiment is described for the introductory organic chemistry laboratory course wherein half of the students use sodium borohydride (NaBH[subscript 4]) and the other half use sodium borodeuteride (NaBD[subscript 4]) to reduce acetophenone to 1-phenylethanol and then compare spectral data. The cost is reasonable, and the experiment is well-suited to serve as a first experience with [superscript 1]H NMR spectroscopy, infrared spectroscopy, and/or mass spectrometry. No special apparatus are required for the reaction. The entire experiment, including an extensive prelab lecture and acquisition of [superscript]1 H NMR data, is completed in a 3 h period. The experiment can stand alone, but lends itself to cross-course collaboration between the organic and physical chemistry laboratories. The succeeding companion article describes the measurement of a kinetic isotope effect using the product from this experiment. The physical chemistry students report their experimental results back to the organic class.