Mesostructured MIL-101 metal-organic framework materials were successfully synthesized by solvothermal process thought controlling molar ratio of chromium (III) nitrate (Cr) to l.4-benzene dicarboxylic acid (H2BDC). The obtained samples were characterized by powder X-ray diffraction, scanning electron microscope (SEM), transmission electron microscope (TEM), thermal analysis (TG-DTA), fourier transform infrared spectroscopy (FT-IR) and nitrogen adsorption/desorption isotherms at 77K. The results showed-that in an approxunate synthetised condition, the MIL-101 with a mesoporous structure and highly crystallized regular octahedron with a perfect cubic symmetry is obtained.