Study of Process for Synthesis of Epoxycyclohexane with t-Butyl Hydroperoxide as Oxidant

A molybdenum(Ⅵ)complex,namely molybdenum dioxobis(2,4 pentanedione)[ MoO 2(acac) 2] ,to be used as epoxidation catalyst was synthesized.It was characterized by elementary analysis and infrared spectrum technique. t Butyl hydroperoxide ( t BuOOH) to be used as epoxidation agent was also synthesized.Under the protection of nitrogen,process of synthesizing epoxycyclohexane by reaction of cyclohexene and t BuOOH using MoO 2(acac) 2 as catalyst was investigated.Possible mechanism of the epoxidation reaction by MoO 2(acac) 2 catalysis was described.Effects of mole ratio of cyclohexene to t BuOOH and amounts of catalyst,solvent etc.on reaction yield were studied by orthogonal experiment design.The optimum reaction conditions were obtained,that is,according to n(t BuOOH) = 0 1 mol, n ()∶ n(t BuOOH)=3 5∶1 0,volume of solvent is about 10 mL,reaction temperature is about 80 ℃,and reaction time is about 60 min.Under these conditions,the yield of epoxycyclohexane based on the amount of t BuOOH is over 99 5%,and purity of epoxycyclohexane is about 99 9% by GC analysis.