Search results for "PALLADIUM"
showing 10 items of 956 documents
Palladium-Catalyzed Synthesis of Mono- and Diphosphorylated 1,10-Phenanthrolines
2012
A general protocol for the coupling of mono- and dihalo-1,10-phenanthrolines with diethyl phosphite is reported. This reaction proceeds smoothly in the presence of a Pd(OAc)2/dppf catalytic system and triethylamine as a base.
Green conditions for the Suzuki reaction using microwave irradiation and a new HNT-supported ionic liquid-like phase (HNT-SILLP) catalyst
2014
A new catalytic system based on modified halloysite nanotubes was employed in the Suzuki reaction under microwave irradiation. A set of solvents, times and bases was screened and the best experimental conditions were obtained when the reactions were carried out for 10 min in water–ethanol at 120 °C in presence of K2CO3 as base. Good recyclability was observed. The new catalytic system was employed using either 1 mol% or 0.1 mol%. The palladium catalyst displayed good activity, allowing the synthesis of several biphenyl compounds in high yield working with only 0.1 mol% palladium loading. The application of microwave irradiation decreased the reaction time and also improved conversion with r…
Bis(oxamato)palladate(II) complexes: synthesis, crystal structure and application to catalytic Suzuki reaction
2015
New bis(oxamato)palladate(II) complexes, [Pd(H2O)4][Pd(2,6-Me2pma)2]·2H2O (1), (n-Bu4N)2[Pd(2,6-Me2pma)2]·2H2O (2a), and (n-Bu4N)2[Pd(2,6-Me2pma)2]·2CHCl3 (2b) (2,6-Me2pma = N-2,6-dimethylphenyoxamate and n-Bu4N+ = tetra-n-butylammonium), have been synthesized and the structures of 1 and 2b characterized by single-crystal X-ray diffraction. Complex 1 is a double salt constituted by tetraaquapalladium(II) cations and bis(oxamato)palladate(II) anions interlinked by hydrogen bonds. The palladium(II) ions in 1 are four-coordinate with two oxygens and two nitrogens from two fully deprotonated oxamate ligands (anion), and four water molecules (cation) building centrosymmetric square-planar surrou…
Isolation of enantiomerically pure organometallic palladium compounds: synthesis of the triangles prepared from enantiopure [cis-Pd2(C6H4PPh2)2(NCCH3…
2009
Reaction of the racemic [Pd(C(6)H(4)PPh(2))Br](4) () with the silver salt of 1R-(1alpha,2beta,3alpha)]-3-methyl-2-(nitromethyl)-5-oxocyclopentaneacetate, (R)-AgO(2)CR*, results in the formation of a mixture of diastereoisomers (RRR)- and (SRR)- of the formula Pd(2)(C(6)H(4)PPh(2))(2)(O(2)CR*)(2) that were separated by standard chromatographic methods. Each diastereoisomer was readily converted into the tetrametallic stereoisomers (SS)- and (RR)-, of the formula [Pd(C(6)H(4)PPh(2))Br](4) that were isolated and characterized by X-ray crystallography. The R enantiomer of the solvated cationic species [cis-Pd(2)(C(6)H(4)PPh(2))(2)(NCCH(3))(4)](2+), obtained from (RR)-, was reacted with ammonium…
Der (2-Phenyl-2-trimethylsilyl)ethyl-(PTMSE)-Ester – eine neutral spaltbare Carboxyschutzgruppe/The (2-Phenyl-2-trimethylsiylyl)ethyl (PTMSE) Ester –…
2002
(2-Phenyl-2-trimethylsilyl)ethyl (PTMSE) esters of aminoacids and peptides are stable under the conditions of hydrogenolytic cleavage of benzoxycarbonyl(Z) and benzyl ester groups, base-induced removal of Fmoc groups, palladium(0)-catalyzed removal of allyloxycarbonyl (Aloc) and even acidolytic cleavage of Boc groups. PTMSE esters are also stable under the conditions of peptide condensation reactions. The PTMSE ester is selectively cleaved by treatment with tetrabutylammonium fluoride (TBAF) trihydrate in dichloromethane, i. e. under almost neutral conditions, within a few minutes and, therefore, considered a valuable novel carboxy protecting group.
Rhodium and palladium complexes from 1,1′ and 1,2 ferrocenylphosphine as bidentate ligands. Versatile coordination
2000
Abstract The complexation of the mixed bidentate ligands 1-diphenylphosphino-1′-diphenylthiophosphinoferrocenyl and 1,2-bis(diphenylphosphino)ferrocenyl with rhodium(I) and palladium(II) species yield a range of mono- and dirhodium or palladium complexes. Their interest as possible catalysts for alkene hydroformylation and alkoxycarbonylation and Heck coupling reactions has been assessed. Fe[C5Me4P(S)Ph2][C5Me4PPh2]PdCl2 and Fe[C5H2-1,2-(PPh2)2-4-tBu][C5H5]PdCl2 have been characterized by single-crystal X-ray diffraction studies.
Functionalized Tri‐ and Tetraphosphine Ligands as a General Approach for Controlled Implantation of Phosphorus Donors with a High Local Density in Im…
2014
Supported phosphine ligands are auxiliaries of topical academic and industrial interest in catalysis promoted by transition metals. However, both controlled implantation and controlled conformation of ligands should be achieved to produce immobilized catalysts that are able to structurally “copy” efficient homogeneous systems. We provide herein a general synthetic strategy for assembling a new class of branched tetra- and triphosphine ligands with a unique controlled rigid conformation, and thus providing a high local density of phosphorus atoms for extended coordination to the metal center. We prepared new functionalized cyclopentadienyl (Cp) salts to design polyphosphines that were “ready…
Organometallic ABC-triblock copolymers
1998
The interaction of Fe and Pd complexes with double bonds of the polybutadiene (PB) block in polystyrene-polybutadiene-poly(methyl methacrylate) block copolymers has been studied. The incorporation of Fe(CO)3 fragments into the PB bloc was found to result in an increase in its rigidity. The presence of iron or palladium complexes in the PB block affects strongly the morphology of the triblock copolymers.
Heterogeneously catalyzed Suzuki-Miyaura conversion of broad scope
2012
The reaction tolerates a broad range of functional groups in the coupling partners and is usually performed in solution under homogeneous conditions at T ¢ 60 uC using 2–3 mol% catalytic amounts. The catalyst is often a Pd(0) complex with triarylphosphane ligands. 2 The catalytic cycle (Scheme 2) begins with the oxidative addition of an aryl halide to a Pd(0) species formed in situ to form an arylpalladium(II) halide intermediate. 3 Chloroarenes, especially nonactivated aryl chlorides, are notoriously less reactive due to the stability of the C–Cl bond (the relative reactivity of Ar–X is correlated to the respective bond dissociation energy: Ph–Cl: 96 kcal mol 21 ,P h–Br: 81 kcal mol 21 ,P …
High Yield Syntheses of Stable, Singly Bonded Pd26+ Compounds
2006
A general method for the syntheses of dipalladium compounds having a singly bonded Pd26+ core and the formula R,S-cis-Pd2(C6H4PPh2)2(O2CR)2Cl2 is described. When the alkyl group in the carboxylate ligands is an electron donating group, the compounds are stable and the yields high. The Pd-Pd distances for the diamagnetic compounds with R = CF3 and CMe3 are 2.5434(4) and 2.5241(9) A, respectively. Calculations at the DFT level suggest that the electronic configuration is sigma2pi4delta2delta*2pi*4. These represent rare examples of palladium(III) compounds.