Mesoporous aluminosilicate (MAS) and bifunctional catalysts based on it were synthesized. The MAS synthesis is based on the method of copolycondensation of silicon and aluminum sources in the presence of alcohol. Hexadecylamine was used as a template for the formation of a porous structure. The catalysts were characterized by X-ray diffraction, Brunauer–Emmett–Teller, temperature-programmed desorption of ammonia, hydrogen-temperature programmed reduction, Fourier transform infra-red spectroscopy, and diffuse reflectance infrared Fourier transform spectroscopic methods. The catalytic activity of Ni/MAS-H-bentonite and Mo/MAS-H-bentonite was investigated during the hydroconversion of n-hexadecane. It has been shown that a sample promoted with molybdenum and nickel based on MAS has the high activity and selectivity in the process of n-hexadecane hydroisomerization under optimal conditions (320°C, atm pressure).