Tetrakis(acetato)dirhodium(II) and Similar Carboxylato Compounds

Abstract

The dimeric tetraacetato bridged Rh2(0COCH3) has been obtained by the interaction of ammonium chlororhodate(II1) or rhodium(II1) hydroxide with acetic a~i d , l -~ Other (carboxylato)rhodium(II) compounds were prepared directly in a similar way or from the acetate by e x~h a n g e .~?~ Halo carboxylates (RCOO-, R = CC13, CF3, CH2C1, etc.) were prepared also by interaction of rhodium trichloride with the appropriate sodium salt in ethan01.~ The carboxylatcs are normally first isolated as a solvent adduct, e.g., [Rh(OCOR) z.CzH50H]2 but are easily converted to the unsolvated complex. The acetate is readily prepared in a modification of this last procedure. A similar method is satisfactory for the preparation of other lower carboxylates as well as halo carboxylates. ProcedureCommercial rhodium trichloride trihydrate (5.0 g.) and sodium acetate trihydrate (10.0 g.) in glacial acetic acid (100 ml.) and absolute ethanol (100 ml.) were gently refluxed under nitrogen for an hour.The initial red solution rapidly becomes green, and a green solid is deposited. After cooling t o room temperature the green

Homoleptic dirhodium tetraoctanoate and its pyridine adduct: synthesis and crystal structures

“…moderate yield (70%) by direct reaction of rhodium trichloride trihydrate with sodium octanoate in the presence of octanoic acid, similar to the preparation of dirhodium tetraacetate described by Rempel et al [23]. Complex 2 was synthesized by the addition of pyridine to an ethanol solution of 1.…”

“…Synthesis of Rh 2 (O 2 CC 7 H 15 ) 4 (1) Rh 2 (O 2 CC 7 H 15 ) 4 was prepared by a similar procedure to that used for dirhodium tetraacetate as described elsewhere [23]. To a mixture of rhodium trichloride trihydrate (1.32 g, 5 mmol) and sodium octanoate (2.49 g, 15 mmol) in 150 mL of absolute alcohol was added octanoic acid (1 mL, 6 mmol).…”

Synthesis and Structural and Physicochemical Characterization of {[Rh2(μ‐OOCCH3)2(dmbpy)2][BF4]}n Molecular Wire

“…The oxidation peak potential of 3 in the solid state [ Figure 5A( 4 ] was prepared as described in the literature. [29] 1 H NMR spectra were measured with a Bruker AMX 300 and Avance 500 spectrometers, IR spectra were measured with a Bruker IFS 113v spectrometer, EPR spectra were obtained with a Bruker ESP 300E and UV/Vis spectra were recorded with a Beckman DU-7500, Cary 5 and Cary 500 spectrometers. The reflectance spectra of the powdered samples of complex 3 were recorded by using MgO as a reference.…”

A facile synthesis of 4-gem-difluoromethylene β-lactam and its derivatives from BrCF2CF2Br

“…Raising the temperature did not enhance the yield obviously. Further experimental tries turned out that it was inert to the other free radical initiating conditions, such as CrCl 3 /Fe, Cp 2 TiCl/Fe, NaS 2 O 4 /NaHCO 3 , CuCl/ethanolamine and Pd [11], etc. (Scheme 5).…”