An efficient, versatile and non-destructive in situ method in reaction monitoring using vibrational spectroscopy is described. A Suzuki cross-coupling reaction was monitored in which the substrate 1-iodo-2-nitrobenzene reacted with the electrophile phenylboronic acid to form the product 2-nitrobiphenyl. To hasten the reaction, palladium(II) acetate and potassium carbonate were added to serve as catalyst and to promote transmetalation, respectively. This reaction was monitored using near-infrared and Raman spectroscopy. The recorded data was subjected to multivariate analysis such as principal component analysis in order to detect spectral changes due to the formation of the product. To confirm the presence of the desired product, offline analyses were performed using gas chromatography-mass spectrometry and nuclear magnetic resonance spectroscopy. The results demonstrate how Raman spectroscopy is able to detect the formation of the product in real time, whereas near-infrared spectroscopy fails to do so.