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- New trendy magnetic C-scorpionate iron catalyst and its performance towards cyclohexane oxidationPublication . Da Costa Ribeiro, Ana Paula; Matias, Inês; Alegria, Elisabete; Ferraria, Ana Maria; Rego, Ana; Pombeiro, Armando; Martins, LuisaFor the first time, a magnetic C-scorpionate catalyst was prepared from the iron(II) complex [FeCl2{_3-HC(pz)3}] (pz = pyrazol-1-yl) and ferrite, using the sustainable mechanochemical synthetic procedure. Its catalytic activity for the cyclohexane oxidation with tert-butyl hydroperoxide (TBHP) was evaluated in different conditions, namely under microwave irradiation and under the effect of an external magnetic field. The use of such magnetic conditions significantly shifted the catalyst alcohol/ketone selectivity, thus revealing a promising, easy new protocol for tuning selectivity in important catalytic processes.
- Comparison of microwave and mechanochemical energy inputs in the catalytic oxidation of cyclohexanePublication . Da Costa Ribeiro, Ana Paula; Alegria, Elisabete; Kopylovich, Maximilian; Ferraria, Ana Maria; Rego, Ana; Pombeiro, ArmandoThe effect of microwave and mechanochemical ball milling energy inputs was studied for the peroxidative oxidation (with aqueous H2O2) of cyclohexane to cyclohexanol and cyclohexanone, over CoCl2 and/or V2O5 dispersed (μm scale) catalysts. A maximum total yield of cyclohexanol and cyclohexanone of 43% after 1 h of reaction at 30 °C, in acetonitrile and under microwave irradiation (5 W), was achieved over the CoCl2–V2O5 (3 : 1) catalyst prepared by ball milling. Cyclohexanol is the main final product with a selectivity of up to 93% over cyclohexanone. Conducting the oxidation reaction under microwave irradiation under the same conditions but without any mechanochemical treatment of the catalyst prior to use resulted in a lower total yield of 30% with a lower selectivity (69%) towards cyclohexanol over cyclohexanone. The sole application of mechanochemical treatment for the catalyst preparation and the catalytic oxidation of cyclohexane allowed to reach yields of 29% after 1 h of reaction, at room temperature, without microwave irradiation and any additive and in the absence of any organic solvent. Ball milling is shown to provide a convenient, solvent-free method to disperse these solid catalysts and to promote the above cyclohexane oxidation, although, in the latter case, not so effectively as microwave irradiation.