Search results for "Iodide"

Screening of ligands for the Ullmann synthesis of electron-rich diaryl ethers

2012

In the search for new ligands for the Ullmann diaryl ether synthesis, permitting the coupling of electron-rich aryl bromides at relatively low temperatures, 56 structurally diverse multidentate ligands were screened in a model system that uses copper iodide in acetonitrile with potassium phosphate as the base. The ligands differed largely in their performance, but no privileged structural class could be identified.

2,2′:6′,2″-Terpyridine Trimethylplatinum(IV) Iodide Complexes as Bifunctional Halogen Bond Acceptors

2016

Three new organometallic trimethylplatinum(IV) iodide complexes of 2,2′:6′,2″-terpyridines have been synthesized and characterized by 1H NMR spectroscopy, mass spectrometry, elemental analysis, and single crystal X-ray diffraction analysis. The X-ray crystal structures of PtMe3I(L) complexes 1–3 {L for 1 = 4′-chloro-2,2′:6′,2″-terpyridine, 2 = 4′-(4-cyanophenyl)-2,2′:6′,2″-terpyridine, and 3 = 4′-(4-tolyl)-2,2′:6′,2″-terpyridine} reveal distorted octahedral coordination geometry of the platinum(IV) metal centers with bidentate coordination of the terpyridine ligands. Complexation of 1–3 with iodopentafluorobenzene (IPFB) afforded single-crystal structures of halogen bond (XB) complexes 1a–3…

Experimental and theoretical investigations of the contact ion pairs formed by reactions of the anions [(EPR2)2N]- (R = (i)Pr, (t)Bu; E = S, Se) with…

2010

Reactions of the sodium salts [(EPR(2))(2)N]Na(TMEDA) (R = (i)Pr, (t)Bu; E = S, Se) with the iodide salts [(TePR(2))(2)N]I (R = (i)Pr, (t)Bu) in toluene produce the mixed-chalcogen systems [(EPR(2))(2)N][(TePR(2))(2)N] (6b, E = Se, R = (t)Bu; 6c, E = S, R = (t)Bu; 7b, E = Se, R = (i)Pr; 7c, E = S, R = (i)Pr). Compounds 6b, 6c, 7b, and 7c have been characterized in solution by variable-temperature multinuclear ((31)P, (77)Se, and (125)Te) NMR spectroscopy and in the solid state by single-crystal X-ray crystallography. The structures are comprised of contact ion pairs linked by bonds between Te and S or Se atoms. For the tert-butyl derivatives 6b and 6c, the anionic half of the molecule is co…

The catalytic-thermometric determination of molybdenum in steels based on the hydrogen peroxide-iodide indicator reaction

1990

Abstract The Mo VI -catalysed hydrogen peroxide-iodide reaction has been optimised for thermometry in an HCl medium using the initial slope method. The substitution of sodium perborate by H 2 O 2 and the conversion of the reaction to a process showing a Landolt effect are considered and discussed. The linear range extended from 0.2 μg Mo VI ml −1 to 1.2 μg Mo VI ml −1 with a detection limit of 0.06 μg Mo VI ml −1 . Interferences were also studied. The optimised procedure was applied to the evaluation of molybdenum in steels after extraction with α-benzoinoxime in chloroform.

Synthese und Reaktionen der 3-O-Phosphoniogluco-und -allofuranosen

1982

Aus den bicyclischen Gluco- (3, 5, 7 und 9) und Allofuranosen 11 werden mit Triphenylphosphan (1), Azodicarbonsaure-diethylester (2) und Alkylierungs- oder Acylierungsmitteln isolierbare 3-O-Phosphoniokohlenhydrate (4, 6, 8, 10 und 12) hergestellt. Durch Erwarmen der allo-konfigurierten Salze 12 konnen an C-3 epimere gluco-konfigurierte Substitutionsprodukte in groser Vielfalt gewonnen werden. Die Reaktionen der gluco-konfigurierten Salze werden stark vom Charakter des einzufuhrenden Nucleophils und von Nachbargruppen im Kohlenhydratgerust beeinflust. Wahrend das Iodid 4a und das Azid 4g unter Substitution zum allo-Derivat 15 reagieren, tritt in den Fallen mit Bromid, Chlorid oder Sulfonat …

2020

Reduction of the aluminum iodide AlI2AriPr8 (1; AriPr8 = C6H-2,6-(C6H2-2,4,6-Pri3)2-3,5-Pri2) with 5% w/w Na/NaCl in hexanes gave a dark red solution from which the monomeric alanediyl :AlAriPr8 (2) was isolated in ca. 28% yield as yellow-orange crystals. Compounds 1 and 2 were characterized by X-ray crystallography, electronic and NMR spectroscopy, and theoretical calculations. The Al atom in 2 is one-coordinate, and the compound displays two absorptions in its electronic spectrum at 354 and 455 nm. It reacts with H2 under ambient conditions to give the aluminum hydride {AlH(μ-H)AriPr8}2, probably via a weakly bound dimer of 2 as an intermediate.

Das System 2‐Halogenethylester/Cholinester als Zweistufen‐Schutzgruppe für die Carboxylfunktion von Aminosäuren und Peptiden

1979

Das System 2-Chlorethyl- und 2-Bromethylester/Cholinester wird als Carbonsaure-Schutzfunktion beschrieben. Die 2-Chlorethyl-(OEt(Cl))- und die 2-Bromethylester (OEt(Br)) der Aminosauren (4) lassen sich einfach herstellen und mit Z- und Boc-Aminosauren zu Z- und Boc-Dipeptidestern 5 und 6 verknupfen. Die Esterfunktionen sind gegen nicht zu stark saure und basische Einflusse bestandig. Sie konnen mit Natriumiodid in DMF in 2-Iodethylester 8 ubergefuhrt werden, welche mit Zink in einer Eintopfreaktion spaltbar sind. Durch Umsetzung mit Trimethylamin gehen die hydrophoben 2-Halogenethylester in die hydrophilen Cholinester 10 und 11 uber. Diese sind sehr stabil gegen Sauren. Sie konnen in wasrig…

Photoiodocarboxylation of Activated C═C Double Bonds with CO2 and Lithium Iodide

2018

The photolysis at 254 nm of lithium iodide and olefins 1 carrying an electron-withdrawing Z-substituent in CO2-saturated (1 bar) anhydrous acetonitrile at room temperature produces the atom efficient and transition metal-free photoiodocarboxylation of the C═C double bond. The reaction proceeds well for terminal olefins 1 to form the new C-I and C-C σ-bonds at the α and β-positions of the Z-substituent, respectively, and is strongly inhibited by polar protic solvents or additives. The experimental results suggest that the reaction channels through the radical anion [CO2•-] in acetonitrile, yet involves different intermediates in aqueous medium. The stabilizing ion-quadrupole and electron don…

Detection and localisation of disulphide bonds in a synthetic peptide reproducing the sequence 1-30 ofPar j1.0101 by electrospray ionisation mass spe…

2001

The structural characterisation of a synthetic peptide reproducingthe sequence 1–30 of Par j 1.0101, a major allergenic protein present in the pollen of Parietaria judaica, by combined use of chemical and enzymatic cleavage, reversed-phase high-performance liquid chromatography (RP-HPLC) and electrospray ionisation mass spectrometry (ESI-MS), is described. Direct ESI-MS of the synthetic peptide after reaction with methyl iodide showed that the product is a mixture of two peptides: one form in which two out of the four cysteine residues present in the sequence are oxidised and a minor amount of another form in which all the cysteines are fully reduced. It was ascertained, usingthe combined p…

Aminoendgruppenhaltige polymere durch anionische polymerisation von vinylverbindungen mit 3-Dimethylaminopropyllithium als initiator

1975

α-Methylstyrol (in THF) sowie Styrol bzw. Butadien (in Benzol) wurden mit 3-Dimethyl-aminopropyllithium (1) als Initiator homopolymerisiert; dabei wurden aufgrund des Einflusses der tertiaren Aminogruppe bei der Polymerisation in apolarem Medium, verglichen mit der Initiierung durch Butyllithium, Veranderungen der Mikrostruktur der Polymeren beodachtet. Die Molekulargewichte der Polymeren sind hoher, als sich nach dem eingesetzten Monomer/Initiator-Verhatnis berechnete. Der Aminoendgruppengehalt der Polymeren wurde elementaranalytisch sowie NMR-spektroskopisch quantitative bestimmt; die tertiaren Aminoendgruppen konnten mit Methylijodid quantitativ zum quartaren Salz umgesetz werden, mit Br…