Raman spectroscopy in conjunction with microwave heating is a convenient and robust tool for monitoring organic reactions from a qualitative perspective. Its validity as a method for obtaining quantitative data is shown. Activation enthalpies for the synthesis of a range of substituted chalcones are determined and the results compared with well-established previous data and reactivity trends for this aldol condensation. The methodology is used for obtaining previously unreported pK(a) data for substituted acetophenones.