Synthesis of Beta zeolite catalysts was carried out using two different methods. The influence of such parameters as synthesis time and temperature, gel composition and gel ripening on the physico-chemical and catalytic properties of Beta zeolite catalysts was studied. A range of analytical methods was applied in this work including scanning and transmission electron microscopies, energy dispersive X-ray spectroscopy, X-ray powder diffraction, nuclear magnetic resonance spectroscopy – 27A1-MAS-NMR and 29Si-MAS-NMR, nitrogen physisorption, Fourier transform infrared spectroscopy and inductively coupled plasma optical emission spectrometry. The sodium forms of Beta zeolites were transformed to the proton forms H-Beta by ion-exchange using aqueous solutions of NH4NO3 and thereafter evaluated in Prins cyclization of (−)-isopulegol with benzaldehyde. The best catalyst synthesized at 150 °C in the rotation mode for 17 h possessing an optimal combination of morphological and structural properties as well as concentration of acid sites demonstrated high (−)-isopulegol conversion (93%) along with high selectivity to the desired product (79%).