Efficient and Rapid Synthesis of Chlorido‐Bridged Half‐Sandwich Complexes of Ruthenium, Rhodium, and Iridium by Microwave Heating

Abstract

The dinuclear complexes [(p‐cymene)RuCl2]2 and [(cyclopentadienyl)MCl2]2 (M = Ru, Rh, Ir) are important starting materials in organometallic chemistry. The standard synthesis of these complexes involves heating of an alcoholic solution of RuIII, RhIII, or IrIII salts with precursors of the π‐ligands for several hours under reflux. Microwave heating allows these complexes to be obtained within a few minutes without compromising the yields. Furthermore, the microwave‐assisted syntheses require less solvent and, in some cases, lower amounts of ligand precursors.

Antitumor pentamethylcyclopentadienyl rhodium complexes of maltol and allomaltol: Synthesis, solution speciation and bioactivity

“…The ligand was deprotonated by sodium methoxide, followed by conversion with the Rh III dimer at room temperature (Scheme 1). The isolated yield was found to be slightly lower (71%) compared to the maltol complex (90% [38] at 140 °C which decreased the reaction time from several hours at reflux to minutes. We decided to investigate the potential of this powerful tool for the synthesis of organorhodium compounds 1a and 1b.…”

Heterogenized Iridium Water-Oxidation Catalyst from a Silatrane Precursor

“…Once the majority of the methanol was removed, the reaction was cooled, filtered, and washed with cold methanol to yield p-tolylsilatrane as a white solid (7.588 g, 29 mmol, 95%). (p-tolyl silatrane) : 1 H NMR (CDCl 3 with 0.05% v/v TMS, 400 MHz): δ 7.65 -7.57 (2H, m, CH), 7.12 -7.04 (2H, m, CH), 3.89 (6H, t, J = 5.9 Hz, CH 2 ), 2.90 (6H, t, J = 5.9 Hz, CH 2 ), 2.27 (3H, d, J = 0.6 Hz, CH 3 ).…”

“…Pentamethylcyclopentadienyl iridium dichloride dimer, (IrCp*Cl 2 ) 2 , 3 3-aminophenylsilatrane, 4 and Cp*Ir(2-(2'-pyridyl)-2-propanolate)Cl (Cp* = pentamethylcyclopentadienyl), 5 were synthesized and characterized by previously reported methods.…”

Half-Sandwich Ru(II) Halogenido, Valproato and 4-Phenylbutyrato Complexes Containing 2,2′-Dipyridylamine: Synthesis, Characterization, Solution Chemistry and In Vitro Cytotoxicity

“…[Ru(µ-Cl)(η 6 -p-cym)Cl] 2 was prepared according to the reported synthetic procedure performed in the microwave reactor [35]. Silver valproate (Ag(VP)) and silver 4-phenylbutyrate (Ag(PB)) were obtained by the neutralization of the methanolic solutions of valproic or 4-phenylbutyric acid with the stoichiometric amount of 1 M NaOH (5 min of stirring at ambient temperature) followed by the addition of 1 molar equivalent of silver triflate (5 min of stirring at ambient temperature in the dark).…”