A concise procedure for the one-step synthesis of isotruxene has been developed. Isotruxene is obtained in around 60% yield on a 150-gram scale through acid-catalysed cyclotrimerisation of equimolar amounts of 1-indanone and 2-indanone. The separation procedure is convenient and is based on different solubilities between isotruxene and side products.
Beyond Takai's Olefination Reagent: Persistent Dehalogenation Emerges in a Chromium(III)-μ3-Methylidyne Complex
Reaction of CHI3 with six equivalents of CrCl2 in THF at low temperatures affords [Cr3Cl3(μ2-Cl)3(μ3-CH)(thf)6] as the first isolable high-yield CrIII μ3-methylidyne complex. Substitution of the terminal chlorido ligands via salt metathesis with alkali-metal cyclopentadienides generates isostructural half-sandwich chromium(III)-μ3-methylidynes [CpR3Cr3(μ2-Cl)3(μ3-CH)] (CpR=C5H5, C5Me5, C5H4SiMe3). Side and decomposition products of the Cl/CpR exchange reactions were identified and structurally characterized for [Cr4(μ2-Cl)4(μ2-I)2(μ4-O)(thf)4] and [(η5-C5H4SiMe3)CrCl(μ2-Cl)2Li(thf)2]. The Cl/CpR exchange drastically changed the ambient-temperature effective magnetic moment μeff from 9.30/9.11 μB (solution/solid) to 3.63/4.32 μB (CpR=C5Me5). Reactions of [Cr3Cl3(μ2-Cl)3(μ3-CH)(thf)6] with aldehydes and ketones produce intricate mixtures of species through oxy/methylidyne exchange, which were partially identified as radical recombination products through GC/MS analysis and 1H NMR spectroscopy.
Anwander, Reiner,Langmann, Jan,Maichle-M?ssmer, C?cilia,Scherer, Wolfgang,Trzmiel, Simon,Werner, Daniel
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p. 20049 - 20054
(2021/08/06)
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