Abstarct: Heterogeneous catalyst have been used extensively for variety of organic reactions. In this research mextal-organic frxamework (MIL-101) with high surfacearea (up to 3000m2/g) and high degree of coordination unsaturated mextal sites (CUS) were prepared by hydrothermal processing. Then it was covalently functionalized with diethylentriamine and molybdenum-oxo-acetylacetonate. This catalyst were analyzed by FT-IR, ICP, TG and SEM and then it was used in epoxidation of Alkenes and yields of products were investigated by GC. The catalytic procedur were optimized for dirfferent parameters such as amount of catalyst, solvent, oxidant, temperature and time. It was found that the optimized conditions with over 95% yield for epoxidation of 0.5 mmol cis-cyclooctene with 15 mg of catalyst were 2ml CCl4 as solvent and 1.12 mmol t-butyl-hydroperoxide as oxidant at 85℃. The maximum yield were obtained after 120min for DETA-MIL-101[MoO2(acac)]. In addition recycling experiments revealed that these catalyst could be repeatedly applied for nearly complete epoxidation of alkenes for at least four successive cycles.