Friedel-Crafts Alkylation of Toluene as a Parallel Reaction in Propylene Dimerization Catalyzed by Nickel β-Diimine Complex/EASC in Homogeneous Phase

Vicente, Isabel; Bernardo-Gusmão, Kátia; Souza, Michèle Oberson de; Souza, Roberto Fernando de

doi:10.5935/0103-5053.20140225

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“…Using a modified protocol of one reported in the literature, 26 we developed a convenient entry to the free-base Me nacnac Ph H in a 47% yield by slowly adding HCl at low temperatures to a mixture of acetylacetone dissolved in aniline. 27 Upon completion of the reaction, the solids must be extracted into CH 2 Cl 2 and neutralized with a saturated aqueous solution of Na 2 CO 3 , and the organic layer separated and then dried with MgSO 4 ; the residue (oily material) is then crystallized from MeOH at −35 °C.…”

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confidence: 99%

Werner-Type Complexes of Uranium(III) and (IV)

et al. 2020

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Transmetalation of the β-diketiminate salt [M][MenacnacPh] (M+ = Na or K; MenacnacPh– = {PhNC(CH3)}2CH–) with UI3(THF)4 resulted in the formation of the homoleptic, octahedral complex [U(MenacnacPh)3] (1). Green colored 1 was fully characterized by a solid-state X-ray diffraction analysis and a combination of UV/vis/NIR, NMR, and EPR spectroscopic studies as well as solid-state SQUID magnetization studies and density functional theory calculations. Electrochemical studies of 1 revealed this species to possess two anodic waves for the U(III/IV) and U(IV/V) redox couples, with the former being chemically accessible. Using mild oxidants, such as [CoCp2][PF6] or [FeCp2][Al{OC(CF3)3}4], yields the discrete salts [1][A] (A = PF6 –, Al{OC(CF3)3}4 –), whereas the anion exchange of [1][PF 6 ] with NaBPh4 yields [1][BPh 4 ].

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Section: ■ Results and Discussionmentioning

confidence: 99%

Werner-Type Complexes of Uranium(III) and (IV)

et al. 2020

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“…The low overall concentration of chain-walking products suggests that reinsertion of the products is slow, also consistent with the high C6:C9 selectivity. Consequently, the resulting product distribution can be analyzed as a product of primary insertion selectivity. − Indeed, we recently showed that ethylene dimerization with 1 proceeds through such a coordination–insertion mechanism . Parsing the product distribution into an insertion tree indicates a mechanistic preference for 2,1- over 1,2-insertion of propylene (Scheme ).…”

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confidence: 99%