Lactose is a disaccharide of importance in humans dietary, food products, and the pharmaceutical industry. From the existing isomeric forms, -lactose is rarely found in nature. Thus, in this work, a simple methodology to obtain anhydrous -lactose ( L) from -lactose monohydrate ( L⋅H 2 O) is presented. The L⋅H 2 O powder was dispersed into a basic alcoholic solution (72 hours), at controlled conditions of temperature (27, 29, 31, and 32 ∘ C), without stirring. The slurry was dried at room temperature and characterized. Fourier transform infrared spectroscopy showed the formation of L for the samples prepared at 29 and 32 ∘ C. Raman spectroscopy confirmed this result and suggested the occurrence of crystalline L. Rietveld refinement of the X-ray diffraction patterns was employed to identify and quantify the composition of the isomers. The samples prepared at 29 and 31 ∘ C showed the formation of pure L, while those at 27 and 32 ∘ C showed the presence of L⋅H 2 O and a mixture of the two isomers, respectively. The morphology of the powders was studied by scanning electron microscopy, observing the formation of irregular shape L⋅H 2 O particles and axe-like L particles. Clearly, with this methodology, it was possible to obtain pure, crystalline, and anhydrous L at mild temperature.