Search results for "NICKEL"

Nickel‐Mediated Photoreductive Cross Coupling of Carboxylic Acid Derivatives for Ketone Synthesis**

2021

A simple photochemical, nickel-catalyzed synthesis of ketones starting from carboxylic acids is presented. Hantzsch-ester (HE) functions as a cheap, green and strong photoreductant upon visible-light excitation to facilitate radical generation and also engages in the Ni-catalytic cycle to restore the reactive species. With this dual role, HE allows for the coupling of a large variety of radicals (1°,2°, benzylic, α-oxy & α-amino) with aroyl and alkanoyl moieties, a new feature in the synthesis of ketones through dual nickel photoredox catalysis. With both precursors deriving from abundant carboxylic acids, this protocol is a welcome addition to the organic chemistry toolbox. The reactio…

N-Glycosylamines of 4,6-O-ethylidene-alpha-D-glucopyranose: synthesis, characterisation and structure of CO2H, Cl and F ortho-substituted phenyl deri…

2000

A saccharide based ligand suitable for metal binding (HLCOOH) has been synthesized using 4,6-O-ethylidene-alpha-D-glucopyranose (4,6-O-EGP) and anthranilic acid. A few analogous glycosylamines with chloro and fluoro ortho substitutions have also been synthesized and characterised. Complexes of HLCOOH with Na+, K+, Mg2+, Ca2+, Ba2+, Cd2+ and Hg2+ have been isolated and characterised fully. The crystal structures of 4,6-O-EGP, the chloro analogue of HLCOOH and the K+ complex of L-COOH are established. The anomeric nature, orientation of the binding core and the co-ordination aspects of K+ have been derived from these structures.

Nickel‐Catalyzed C(sp2)−C(sp3) Kumada Cross‐Coupling of Aryl Tosylates with Alkyl Grignard Reagents

2019

Aryl tosylates are an attractive class of electrophiles for cross‐coupling reactions due to ease of synthesis, low price, and the employment of C−O electrophiles, however, the reactivity of aryl tosylates is low. Herein, we report the Ni‐catalyzed C(sp2)−C(sp3) Kumada cross‐coupling of aryl tosylates with primary and secondary alkyl Grignard reagents. The method delivers valuable alkyl arenes by cross‐coupling with challenging alkyl organometallics possessing β‐hydrogens that are prone to β‐hydride elimination and homo‐coupling. The reaction is catalyzed by an air‐ and moisture stable‐Ni(II) precatalyst. A broad range of electronically‐varied aryl tosylates, including bis‐tosylates, underwe…

Physico-chemical investigation of nanostructures in liquid phases: Nickel chloride ionic clusters confined in sodium bis(2-ethylhexyl) sulfosuccinate…

2009

The confinement of finite amounts of nickel chloride in the hydrophilic core of sodium bis(2-ethylhexyl) sulfosuccinate (AOT) reverse micelles dispersed in n-heptane has been investigated by FT-IR, UV-vis-NIR and fluorescence spectroscopies. The analysis of experimental data consistently leads to hypothesize that NiCl(2) forms small size ionic clusters stabilized by a monolayer of oriented surfactant molecules. Due to confinement and interfacial effects, these ionic clusters show peculiar photophysical properties, which are different from those possessed by the bulk material. From NiCl(2)/AOT/n-heptane solutions, by evaporation of the organic solvent, interesting salt/surfactant nanocomposi…

Cobalt(II), nickel(II) and copper(II) complexes withN-cyano-N?-methyl-N?(2-[(5-methyl-1H-imidazol-4-yl)methylthio]ethyl)guanidine

1985

N-Cyano-N′-methyl-N″(2-[(5-methyl-1H-imidazol-4-yl)-methylthio] ethyl) guanidine cimetidine (CM), complexes with CoII, NiII and CuII are described. The compounds are of stoichiometry [M(CM)2]SO4 · nH2O [M = CoII, NiII or CuII; n = 3,3 or 4, respectively], [M(CM)2](ClO4)2 [M = CoII or NiII], [M(CM)2]Cl2 · nH2O [M=CoII, NiII or CuII; n = 1, 2, or 2, respectively] and [Cu(CM)SO4] · 2H2O. The electronic spectra of the compounds in solid state, magnetic susceptibilities and i.r. and e.p.r. spectra were studied. Octahedral environments are proposed for the complexes: [M(CM)2]SO4·nH2O, [M(CM)2](ClO4)2, [Ni(CM)2]Cl2 · 2H2O, [Cu(CM)2]Cl2 · 2H2O and [Cu(CM)SO4] · 2H2O and a tetrahedral structure for …

A Three-Dimensional Homometallic Molecular Ferrimagnet

2002

Coordination chemistry of sulfamethizole: crystal structures of [Cu(sulfamethizolate)2(py)2(OH2)]·H2O, [M(sulfamethizolate)2(py)2(OH2)2] [M=Co and Ni…

2000

Abstract The synthesis and characterisation of copper, cobalt, nickel and zinc compounds with sulfamethizole (4-amino-N-(5-methyl-1,3,4-thiadiazole-2-yl)sulfanilamide) (Hsmtz) are described. The first crystal structures of ternary sulfamethizole complexes are reported. The crystal structures of Cu(smtz)2(py)2(OH2)·H2O (1), M(smtz)2(py)2(OH2)2 [M=Co (2), Ni (3)] and {Cu(smtz)2(dmf)2}∞ (5) were determined by X-ray diffraction. The Cu(II) ion exhibits a square pyramidal geometry in complex 1, while in the other compounds the metal ion presents a distorted octahedral environment. In compounds 1, 2 and 3 the deprotonated sulfamethizole acts as monodentate ligand coordinating through the thiadiaz…

In vitro evaluation of leishmanicidal properties of a new family of monodimensional coordination polymers based on diclofenac ligand

2020

Some series of isostructural chains with general formula [M(diclof)(HO)]·(EtOH) have been obtained from reaction between diclofenac ligand (diclof) and first row transition salts (M = Mn (1),Ni (2) and Co (3)). These monodimensional coordination polymers have been characterized and their crystal structures have been solved by X-ray diffraction methods, elucidating isostructural compounds that are chains with water molecules acting as bridge between different metallic centers, while diclofenac ligands are coordinated to the octahedral coordination environment of the same. Magnetic studies of these complexes have revealed the existence of moderate ferromagnetic interactions among manganese, n…

2-Chloro/phenyl-7-arylimino-6,6-dimethylcyclopenta[b]pyridylnickel chlorides: Synthesis, characterization and ethylene oligomerization

2017

Abstract 2-Chloro/phenyl-7-arylimino-6,6-dimethylcyclopenta[b]pyridylnickel chlorides (Ni1–Ni8) were synthesized from the respective ligands L1–L8 and characterized. Upon activation with either methylaluminoxane (MAO) or ethylaluminium sesquichloride (EASC), they show high catalytic activity of up to 10.84 × 106 g(oligomer) mol− 1(Ni) h− 1 in ethylene oligomerization. The products range from butenes to dodecenes for Ni1–Ni4, but are limited to butenes and hexenes in the case of Ni5–Ni8. DFT calculations indicate that the Ni C bond length in the model alkyl complexes depends both on the nature of the substituents at the heterocycles and the kind of the alkyl group, shedding some light on the…

Synthesis and Reaction Chemistry of Sb(ECH2CH2NMe2)3(E= O, S)

2012

The antimony aminoalkoxide and aminothiolates Sb(ECH 2CH 2NMe 2) 3 [E = O (1), S (2)] were synthesized and their ability to form adducts with other metal moieties investigated. Compound 1 forms 1:1 adducts with NiI 2 (3) and M(acac) 2 [M = Cd (4), Ni (5)], while 2 undergoes ligand exchange with AlMe 3 to afford Me 2AlSCH 2CH 2NMe 2 (6). The structures of 2-4 and 6 were determined. Compound 2 incorporates three S, N-chelating ligands though the interaction with nitrogen is weaker than in analogous alkoxide complexes. Product 3 reveals one iodine has migrated from nickel to antimony, and all three alkoxide ligands bridge the two metals through μ 2-O atoms. In contrast, in 4, only one alkoxide…