Rhenium complexes of P,P,P′,P′-tetrakis(o-hydroxyphenyl)diphosphinoethane

1996 ◽  
Vol 74 (5) ◽  
pp. 722-729 ◽  
Author(s):  
Hongyan Luo ◽  
Chris Orvig
Keyword(s):  
Mass Spectrometry ◽  
Infrared Spectroscopy ◽  
Key Words ◽  
Elemental Analysis ◽  
Ligand Exchange ◽  
Nmr Spectra ◽  
Rhenium Complexes ◽  
Hydrochloride Salt ◽  
H Nmr ◽  
Hexadentate Ligand

Preparation of the hydrochloride salt of a new potentially hexadentate ligand precursor P,P,P′,P′-tetrakis(o-hydroxyphenyl)diphosphinoethane dihydrochloride (abbreviated H4P2O4•2HCl) is described. From H4P2O4•2HCl, neutral [Re2O2Cl2(PPh3)2(μ-P2O4)] and dianionic [Re2O2Br4(μ-P2O4)]2− dinuclear rhenium(V) complexes were synthesized. The complexes have been characterized by elemental analysis, infrared spectroscopy, mass spectrometry, and 1H/31P{1H} NMR spectra. 31P{1H} NMR revealed that only one isomer, presumably the anti, was present for [Re2O2Cl2(PPh3)2(μ-P2O4)], and that two isomers, both anti and syn isomers, were observed for [Re2O2Br4(μ-P2O4)]2−. The coligands (PPh3 for the former, Br− for the latter) of both complexes underwent ligand exchange with pyridine. Key words: rhenium, P,P,P′,P′-tetrakis(o-hydroxyphenyl)diphosphinoethane, dimer, isomers.

Synthesis and Antituberculotic Activity of Some Substituted 3-Arylamino-5-cyano-2-pyrazinecarboxamides

1995 ◽  
Vol 60 (7) ◽  
pp. 1236-1241 ◽  
Author(s):  
Martin Doležal ◽  
Jiří Hartl ◽  
Antonín Lyčka ◽  
Vladimír Buchta ◽  
Želmíra Odlerová
Keyword(s):  
Nucleophilic Substitution ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
Substituted Anilines ◽  
H Nmr

Nucleophilic substitution of 3-chloro-5-cyano-2-pyrazinecarboxamide by substituted anilines afforded substituted 3-arylamino-5-cyano-2-pyrazinecarboxamides I-X. The structures of compounds were confirmed by elemental analysis, UV, IR and 1H NMR spectra. The assessment of in vitro antimycotic and antimycobacterial activities of the compounds was carried out. The highest antituberculotic activity against M. tuberculosis in this series was shown by 3-anilino- 5-cyano-2-pyrazinecarboxamide (I), whose efficacy was the same as that of pyrazinecarboxamide.

scholarly journals Linkage of α-cyclodextrin-terminated poly(dimethylsiloxanes) by inclusion of quasi bifunctional ferrocene

2013 ◽  
Vol 9 ◽  
pp. 1278-1284 ◽  
Author(s):  
Helmut Ritter ◽  
Berit Knudsen ◽  
Valerij Durnev
Keyword(s):  
Electron Microscopy ◽  
Mass Spectrometry ◽  
Light Scattering ◽  
Ir Spectroscopy ◽  
Nmr Spectra ◽  
H Nmr ◽  
Scattering Measurements ◽  
End Groups ◽  
2D Roesy ◽  
2D Roesy Nmr

We report the noncovalent linkage of terminally substituted oligo(dimethylsiloxanes) bearing α-cyclodextrins (α-CD) as host end groups for the cyclopentadienyl rings of ferrocene. This double complexation of unsubstituted ferrocene leads to a supramolecuar formation of the siloxane strands. Structural characterization was performed by the use of 1H NMR and IR spectroscopy and by mass spectrometry. Electron microscopy studies and dynamic light scattering measurements show a significant decrease of the derivative size after the complexation with ferrocene. In addition, further evidence for the successful complexation of the end groups was verified by the shifts of the protons in the 1H NMR spectra and in the correlation signals of the 2D ROESY NMR spectra.

Rhodium(I)–(N-heterocyclic carbene)–diphosphine complexes

2009 ◽  
Vol 87 (9) ◽  
pp. 1248-1254 ◽  
Author(s):  
Hongsui Sun ◽  
Xiao-Yan Yu ◽  
Paolo Marcazzan ◽  
Brian O. Patrick ◽  
Brian R. James
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Benzene Solution ◽  
H Nmr ◽  
Diphosphine Dioxide

Reactions of [RhCl(COE)(IPr)]2 (1) and [RhCl(COE)(IMes)]2 (2) (COE = cyclooctene; IPr = N,N′-bis(2,6-diisopropylphenyl)imidazolin-2-ylidene; IMes = N,N′-bis(2,4,6-trimethylphenyl)imidazolin-2-ylidene) with the diphosphines Ph2P(CH2)nPPh2 and 1,2-bis(diphenylphosphino)benzene (dppbz) give the N-heterocyclic carbene (NHC) – diphosphine – rhodium(I) complexes: RhCl(NHC)[Ph2P(CH2)nPPh2] [NHC = IPr, n = 1 (3); NHC = IMes, n = 1 (4); NHC = IPr, n = 2 (5); NHC = IMes, n = 2 (6); NHC = IPr, n = 4 (7); NHC = IMes, n = 4 (8)] and RhCl(NHC)(dppbz) [NHC = IPr (9); NHC = IMes (10)]. All the complexes are characterized by 1H, 31P{1H}, and 13C{1H} NMR spectroscopy, elemental analysis, and mass spectrometry. Complexes 3, 7, and 9 are also characterized crystallographically. In benzene solution, the complexes decompose in the presence of O2 with formation of the diphosphine dioxide, whereas reaction with CO leads to replacement of the NHC ligand to give known carbonyl–diphosphine complexes.

Reactions of n-C5H5Co(CO)2 and n-Me3SiC5H4Co(CO)2 with (XCN)2 and X(CN)2 (X = S or Se)

1982 ◽  
Vol 37 (3) ◽  
pp. 292-298 ◽  
Author(s):  
Moisés Morán ◽  
Augusto Ibáñez
Keyword(s):  
Elemental Analysis ◽  
Nmr Spectra ◽  
Polar Solvents ◽  
Mixed Complexes ◽  
H Nmr ◽  
Linkage Isomerism

Abstract The pseudohalogens (XCN)2 (X = S or Se) react with n-C5H5Co(CO)2 and n-Me3SiC5H4Co(CO)2 with formation of the 18 electron complexes, RCo(CO)(XCN)2 (R = n-C5H5 or n-Me3SiC5H4). By reactions with X(CN)2 (X = S or Se), the cyclopentadienyl cobalt dicarbonyls are transformed into the mixed complexes, RCo(CO)(CN)(XVN) (R = n-C5H5 or n-Me3SiC5H4. All the compounds are characterized by elemental analysis, IR, electronic and 1H NMR spectra. The thiocyanogen derivatives undergo linkage isomerism (N→S) in polar solvents.

A Novel Reductive Cross-coupling Reaction of 2-nitrobenzoic Hydrazides and Aldehydes or Ketones Promoted by the Low-valence Titanium Reagent: An Access to 2,3,4,5-tetrahydro-1H-1,3,4-benzotriazepine-5-one Derivatives

2005 ◽  
Vol 2005 (9) ◽  
pp. 553-555 ◽  
Author(s):  
Daqing Shi ◽  
Chunling Shi ◽  
Liangce Rong ◽  
Juxian Wang ◽  
Qiya Zhuang ◽  
...  
Keyword(s):  
Elemental Analysis ◽  
Nmr Spectra ◽  
Coupling Reaction ◽  
Cross Coupling ◽  
Reductive Coupling ◽  
Facile Synthesis ◽  
H Nmr ◽  
Cross Coupling Reaction

A short and facile synthesis of a series of 2,3,4,5-tetrahydro-1H-1,3,4-benzotriazepine-5-one derivatives was accomplished in good yields via the intermolecular reductive coupling reaction of 2-nitrobenzoic hydrazides and aldehydes or ketones promoted by the low-valence titanium reagent (TiCl4/Zn system). Structures were established on the basis of elemental analysis, IR and 1H NMR spectra.

scholarly journals N-(tert-Butyldimethylsilyl)imidazole and related heterocycles: 13C nuclear magnetic resonance study and reaction with dimethylsulfoxide

1980 ◽  
Vol 58 (1) ◽  
pp. 60-64 ◽  
Author(s):  
Alexander F. Janzen ◽  
Gerald N. Lypka ◽  
Roderick E. Wasylishen
Keyword(s):  
Mass Spectrometry ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
Elevated Temperatures ◽  
Proton Nmr ◽  
Nuclear Magnetic Resonance Study ◽  
Magnetic Resonance Study ◽  
13C Nuclear Magnetic Resonance ◽  
Methyl Derivatives ◽  
Derivatives Of

N-tert-Butyldimethylsilyl derivatives of imidazole, 2-methylimidazole, 4-methylimidazole, benzimidazole, pyrazole, 1,2,4-triazole, and benzotriazole were prepared from tert-butyldimethylsilyl chloride and the corresponding heterocyclic compound. The products were identified by carbon and proton nmr, mass spectrometry, and elemental analysis. The carbon nmr spectra confirmed the absence of intermolecular silyl exchange at ambient temperature. Silyl exchange did occur at elevated temperatures, 130–160 °C.Reaction of N-tert-butyldimethylsilyl or N-trimethylsilyl heterocycles with dimethylsulfoxide gave N-(methylthio)methyl derivatives of imidazole, 2-methylimidazole, 4-methylimidazole, benzimidazole, pyrazole, and 1,2,4-triazole. The products were characterized by carbon and proton nmr, mass spectrometry, and elemental analysis. A mechanism involving a Pummerer rearrangement is proposed to account for the results.

N-Tribromphosphazo-Verbindungen / N-Tribromophosphaza-compounds

1971 ◽  
Vol 26 (2) ◽  
pp. 75-78 ◽  
Author(s):  
Herbert W. Roesky ◽  
Graalf Remmers
Keyword(s):  
Ir Spectra ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
Chemical Behavior ◽  
H Nmr

By reaction of N-sulfuroxideimides with phosphorus-pentabromide the compounds R-SO2NPBr3 (R = CH3 , CF3 , C6H5, p-Cl-C6H4, and p-CH3C6H4) were prepared. Reactions of hexamethyldisilazane and N- (dimethyl) -trimethylsilylamide resulted in the formation of R-SO2NPBr2N (CH3)2, (R = CH3, C6H5), and R-SO2NPBr2NHSi(CH3)3 (R = CF3, p-CH3-C6H4). The properties and the chemical behavior of these compounds are described. Results of IR-spectra, as well as 31P-, 19F-, and 1H-NMR-spectra and elemental analysis characterize the compounds.

1,1,2,3,4,5 - Hexahydro Tellurophene [C4H8Te(II)] and 1,3-Dihydro-2λ4-Benzotellurole [C8H8Te(II)] Derivatives

2015 ◽  
Vol 7 (1) ◽  
Author(s):  
Rajesh Kumar ◽  
Sangeeta Bajpai
Keyword(s):  
Spectral Data ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
Oxidative Addition ◽  
Addition Reactions ◽  
Tellurium Atom ◽  
Oxidation Number ◽  
H Nmr ◽  
Data Table ◽  
Convenient Route

Convenient route of synthesis of the type R<sub>2</sub>TeX′SY and R<sub>2</sub>Te(CH<sub>3</sub>)X′c were dove loved by the reactions of R<sub>2</sub>Te(II) [R<sub>2</sub> = C<sub>4</sub>H<sub>8</sub>, C<sub>8</sub>H<sub>8</sub>] with IX′S (X′S= Cl, Br), RI (R = CH<sub>3</sub>, C<sub>2</sub>H<sub>5</sub>) and CH<sub>3</sub>X″c (X″c = Cl, Br, NO<sub>3</sub>, C<sub>6</sub>H<sub>5</sub>OCO).These complexes have been characterised through elemental analysis (Table 1) and <sup>1</sup>H NMR spectral data (Table 2). The <sup>1</sup>H NMR spectra of C<sub>4</sub>H<sub>8</sub>TeICl, C<sub>4</sub>H<sub>8</sub>TeIBr, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>I, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>Cl, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>Br, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>NO<sub>3</sub>, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>OCOC<sub>6</sub>H<sub>5</sub>, C<sub>8</sub>H<sub>8</sub>TeCH<sub>3</sub>I, and C<sub>8</sub>H<sub>8</sub>Te -C<sub>2</sub>H<sub>5</sub>I have been recorded in CDCl<sub>3</sub> at 300 MHz. The study indicates that the heterocycles of C<sub>4</sub>H<sub>8</sub>Te(II) and C<sub>8</sub>H<sub>8</sub>Te(II) undergo oxidative addition reactions readily resulting in the increase in the oxidation number of central tellurium atom.

Wolfram-Carbonylkomplexe mit Stickstoff-Wasserstoff-Liganden [1] / Tungsten Carbonyl Complexes with Nitrogen Hydride Ligands [1]

1978 ◽  
Vol 33 (5) ◽  
pp. 542-553 ◽  
Author(s):  
Dieter Sellmann ◽  
Alfred Brandl ◽  
Ralf Endeil
Keyword(s):  
Ligand Exchange ◽  
Nmr Spectra ◽  
Base Catalysis ◽  
Coupling Constants ◽  
Carbonyl Complexes ◽  
H Nmr ◽  
Nitrogen Hydride ◽  
Tungsten Carbonyl ◽  
Synthesis Properties ◽  
Hydride Ligands

Abstract Synthesis, properties and reactions of [(OC)5W]2N2H2, [(OC)5W]2N2H4, (OC)5WN2H4, (OC)5WNH3, [(OC)4PØ3W]2N2H4, [(OC)4PØ3WN2H4], [(OC)5W-N2H2-W(CO)4PØ3], [(OC)5W-N2H2-W(CO)4P(CH3)3] and [(OC)5WNHCH3NHC6H5] are reported. The hydrazine complexes are synthesized by ligand exchange from the corresponding tetra-hydrofuran complexes. Oxidation by various oxidizing agents yields the diazene complexes, in most cases very low yields. Substitution of CO by phosphanes leads to reduced stability of the compounds. All complexes undergo base catalysed H-D exchange yielding the corresponding ND derivatives; the diazene complexes show a much faster exchange than the corresponding hydrazine and ammonia complexes, which is explained by the higher acidity of the N2H2 protons. The diazene complexes disproportionate under base catalysis to hydrazine and dinitrogen compounds, the latter of which loose the N2 ligand immediately. The diazene ligand of [(OC)5W]2N2H2 cannot be alkylated by reactions with (CH3)2SO4, LiCH3 or CH2N2; instead, LiCH3 as well as CH2N2 cause disproportionation to N2H4 and N2 complexes. UV irradiation of [(OC)5W]2N2H2 in THF leads to substitution of CO by THF. The THF complexes can be converted to the phosphane substituted diazene complexes. The IR, UV-VIS and 1H NMR spectra of the (OC)5W complexes are nearly identical to those of the analogous Cr and Mo compounds. The unsymmetrical phosphane diazene complexes, however, show a quartet of the N2H2 protons in the 1H NMR spectra with coupling constants of 25-26 Hz for the protons on the NN double bond. This value points to a trans configuration of the diazene ligand and its complexes respectively.

scholarly journals Nanoparticles of novel organotin(IV) complexes bearing phosphoric triamide ligands

2013 ◽  
Vol 4 ◽  
pp. 94-102 ◽  
Author(s):  
Zahra Shariatinia ◽  
Ebadullah Asadi ◽  
Vahid Tavasolinasab ◽  
Khodayar Gholivand
Keyword(s):  
Fluorescence Spectroscopy ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
Fluorescence Spectra ◽  
Sem Micrographs ◽  
H Nmr ◽  
Phosphoric Triamide ◽  
C Nmr

Four novel organotin(IV) complexes containing phosphoric triamide ligands were synthesized and characterized by multinuclear (1H, 31P, 13C) NMR, infrared, ultraviolet and fluorescence spectroscopy as well as elemental analysis. The 1H NMR spectra of complexes 1–4 proved that the Sn atoms adopt octahedral configurations. The nanoparticles of the complexes were also prepared by ultrasonication, and their SEM micrographs indicated identical spherical morphologies with particles sizes about 20–25 nm. The fluorescence spectra exhibited blue shifts for the maximum wavelength of emission upon complexation.

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