Cyclopentadienyl ruthenium complexes. Part III. Reactivity of some η5-cyclopentadienylbis(triphenylphosphine)ruthenium(II) complexes with nitrosyl tribromide and dinitrogen trioxide

1985 ◽  
Vol 63 (4) ◽  
pp. 963-970 ◽  
Author(s):  
R. F. N. Ashok ◽  
M. Gupta ◽  
K. S. Arulsamy ◽  
U. C. Agarwala
Keyword(s):  
Spectral Data ◽  
Magnetic Moment ◽  
Metal Ion ◽  
Ruthenium Complexes ◽  
General Reaction ◽  
Spectroscopic Evidence ◽  
H Nmr ◽  
Nitrosyl Complexes ◽  
Phenyl Rings ◽  
Triphenylphosphine Ligand

Mixed ruthenium(II) nitrosyls have been synthesized in yields larger than 60% by a general reaction of [Ru(η5-C5H5)(PPh3)L]+X− (L = 2,2′-bipyridine or 1,10-phenanthroline, X = Cl or Br) or [Ru(η5-C5,H5)(PPh3)(L)X] (L = PPh3, pyridine, 3-picoline, 4-picoline, [Formula: see text], or [Formula: see text]; X− = Cl−, Br−, I−, CN−, NCS−, H−, or SnCl3−) with NOBr3 and N2O3. In these complexes NO seems to bind with the metal ion as NO+. The reactions of N2O3 gave either nitrito or nitrosyl dinitrito complexes. The reactions of NOBr3 with trichlorostannate complexes did not yield nitrosyl complexes, instead nitrito complexes were isolated in which spectroscopic evidence (ir, 1H nmr) suggest π-interaction of one of the phenyl rings of the triphenylphosphine ligand to the ruthenium center. All products are characterised by elementary microanalyses, conductivity, magnetic moment measurements, electronic, ir, and 1H nmr spectral data.

Synthesis, characterization and solvent/structural effects on spectral and redox properties of cobalt triphenylcorroles in nonaqueous media

2012 ◽  
Vol 16 (07n08) ◽  
pp. 958-967 ◽  
Author(s):  
Shi Huang ◽  
Yuanyuan Fang ◽  
Aixiang Lü ◽  
Guifen Lu ◽  
Zhongping Ou ◽  
...  
Keyword(s):  
Electron Transfer ◽  
Electrochemical Techniques ◽  
Axial Ligand ◽  
Transfer Reactions ◽  
Redox Potentials ◽  
Nonaqueous Media ◽  
H Nmr ◽  
Chlorinated Solvent ◽  
Phenyl Rings ◽  
Triphenylphosphine Ligand

Five cobalt(III) triphenylcorroles with different electron-withdrawing or electrondonating substituents and an axially bound triphenylphosphine ligand were synthesized and characterized by spectroscopic and electrochemical techniques. The investigated compounds are represented as (4-XPh)3CorCo(PPh3), where Ph3Cor is the trianion of a triphenylcorrole and X is a OMe , Me , H , F or Cl substituent on the meso-phenyl rings. Each corrole was examined by UV-vis, 1H NMR and IR spectroscopy, mass spectrometry, electrochemistry and thin-layer spectroelectrochemistry. Redox potentials and spectra of each oxidized and reduced species were examined in dichloromethane and N,N′-dimethylformamide containing 0.1 M tetra-n-butylammonium perchlorate. Each Co(III) corrole undergoes up to five one-electron transfer reactions, some of which are reversible and others which are not. The CoIII/CoII process is irreversible in both solvents due to the loss of the triphenylphosphine axial ligand following electron transfer. The CoII/CoI process is reversible in DMF but irreversible in CH2Cl2 due to a homogenous chemical reaction between the electrogenerated Co(I) corrole and the chlorinated solvent. The potential for the first oxidation of the investigated corroles varies little with change of solvent, consistent with the lack of solvent binding to the neutral and singly oxidized forms of (4-XPh)3CorCo(PPh3). However, a single DMF molecule strongly binds to the doubly oxidized corrole in DMF or DMF/ CH2Cl2 mixtures. This results in an easier oxidation and a negative shift of ~200 mV in E1/2 upon going from CH2Cl2 to DMF as solvent. The effect of substitutents and solvent on redox potentials is discussed and an overall electroreduction/electrooxidation mechanism is proposed

Synthesis of 2-amino-5,7-dimethyl-4-oxopyrido[3,4-e]-1,3-thiazines

1983 ◽  
Vol 48 (12) ◽  
pp. 3426-3432 ◽  
Author(s):  
Dušan Koščík ◽  
Pavol Kristian ◽  
Ondrej Forgáč
Keyword(s):  
Spectral Data ◽  
Chlorine Atom ◽  
Mass Spectra ◽  
High Reactivity ◽  
Secondary Amines ◽  
Dimroth Rearrangement ◽  
H Nmr ◽  
New Synthesis ◽  
C Nmr

New synthesis of pyrido[3,4-e]-1,3-thiazines consisting in reaction of 2,6-dimethyl-4-chloronicotinoyl isothiocyanate with primary or secondary amines, or with benzaldehyde phenylhydrazone, is described. High reactivity of the chlorine atom does not allow isolation of the corresponding thioureas, arising as intermediates, except in the case of the benzylamino derivative. Structure of the products was unequivocally confirmed by their spectral data (IR, UV, 1H NMR, 13C NMR and mass spectra). The synthesized derivatives do not undergo the Dimroth rearrangement.

Azaoxa Macrocyclic and Acyclic Complexesof Lanthanides

1998 ◽  
Vol 63 (3) ◽  
pp. 363-370 ◽  
Author(s):  
Violetta Patroniak-Krzyminiewska ◽  
Wanda Radecka-Paryzek
Keyword(s):  
Schiff Base ◽  
Spectral Data ◽  
Macrocyclic Ligand ◽  
Lanthanide Ions ◽  
H Nmr ◽  
Elemental Analyses ◽  
Acyclic Complexes ◽  
Schiff Base Cyclocondensation

The template reactions of 2,6-diacetylpyridine with 3,6-dioxaoctane-1,8-diamine in the presence of dysprosium(III), thulium(III) and lutetium(III) chlorides and erbium(III) perchlorate produce the complexes of 15-membered macrocyclic ligand with an N3O2 set of donor atoms as a result of the [1+1] Schiff base cyclocondensation. In contrast, analogous reactions involving the lighter lanthanide ions (lanthanum(III), samarium(III) and europium(III)) yield the acyclic complexes with terminal acetylpyridyl groupings as products of the partial [2+1] condensation. The complexes were characterized by spectral data (IR, UV-VIS, 1H NMR, MS), and thermogravimetric and elemental analyses.

21,22-Disubstituted 18α,19βH-Ursane Derivatives with Oxabicyclooctane System in Ring E

1993 ◽  
Vol 58 (1) ◽  
pp. 173-190 ◽  
Author(s):  
Eva Klinotová ◽  
Jiří Klinot ◽  
Václav Křeček ◽  
Miloš Buděšínský ◽  
Bohumil Máca
Keyword(s):  
Spectral Data ◽  
Spin Systems ◽  
Coupling Constants ◽  
Complete Analysis ◽  
Nmr Spectrum ◽  
Proton Proton ◽  
H Nmr ◽  
Proton Coupling ◽  
C Nmr

Reaction of 3β-acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) and 20β,28-epoxy-21,22-dioxo-19α,19βH-ursan-3β-yl acetate (IIIb) with diazomethane afforded derivatives XII-XIV with spiroepoxide group in position 21 or 22, which were further converted into hydroxy derivatives XV and XVII. Ethylene ketals VIII-X were also prepared. In connection with the determination of position and configuration of the functional groups at C(21) and C(22), the 1H and 13C NMR spectral data of the prepared compounds are discussed. Complete analysis of two four-spin systems in the 1H NMR spectrum of bisethylenedioxy derivative Xb led to the proton-proton coupling constants from which the structure with two 1,4-dioxane rings condensed with ring E, and their conformation, was derived.

scholarly journals Synthesis and antioxidant properties of 2-(3-(hydroxyimino)methyl)-1H-indol-1-yl)acetamide derivatives

2020 ◽  
Vol 6 (1) ◽  
Author(s):  
Chandravadivelu Gopi ◽  
Magharla Dasaratha Dhanaraju
Keyword(s):  
Antioxidant Activity ◽  
Condensation Reaction ◽  
Antioxidant Properties ◽  
Side Chain ◽  
Antioxidant Power ◽  
H Nmr ◽  
Antioxidant Agents ◽  
Phenyl Rings ◽  
Ferric Reducing Antioxidant Power ◽  
Ft Ir

Abstract Background The main aim of this work was to synthesise a novel N-(substituted phenyl)-2-(3-(hydroxyimino) methyl)-1H-indol-1-yl) acetamide derivatives and evaluate their antioxidant activity. These compounds were prepared by a condensation reaction between 1H-indole carbaldehyde oxime and 2-chloro acetamide derivatives. The newly synthesised compound structures were characterised by FT-IR, 1H-NMR, mass spectroscopy and elemental analysis. Furthermore, the above-mentioned compounds were screened for antioxidant activity by using ferric reducing antioxidant power (FRAP) and 1,1-diphenyl-2-picrylhydrazyl (DPPH) methods. Result The antioxidant activity result reveals that most of the compounds were exhibiting considerable activity in both methods and the values are very closer to the standards. Among the synthesised compounds, compound 3j, 3a and 3k were shown remarkable activity at low concentration. Conclusion Compounds 3j, 3a and 3k were shown highest activity among the prepared analogues due to the attachment of halogens connected at the appropriate place in the phenyl ring. Hence, these substituted phenyl rings considered as a perfect side chain for the indole nucleus for the development of the new antioxidant agents.

Evaluation of Antinociceptive and Anti-Inflammatory Activities of a New Triterpene Saponin from Bauhinia variegata Leaves

2009 ◽  
Vol 64 (11-12) ◽  
pp. 798-808 ◽  
Author(s):  
Mona A. Mohamed ◽  
Madeha R. Mammoud ◽  
Heiko Hayen
Keyword(s):  
High Resolution ◽  
Spectral Data ◽  
Cinnamic Acid ◽  
Cinnamic Acid Derivatives ◽  
Triterpene Saponin ◽  
H Nmr ◽  
Antischistosomal Activity ◽  
Bauhinia Variegata ◽  
Anti Inflammatory ◽  
C Nmr

A new triterpene saponin, named as 23-hydroxy-3α-[O-α-L-1C4-rhamnopyranosyl-(1´´4´)- O-α-L-4C1-arabinopyranosyl-oxy]olean-12-en-28-oic acid O-α-L-1C4-rhamnopyranosyl- (1´´´´´→4´´´´)-O-β-D-4C1-glucopyranosyl-(1´´´´→6´´´)-O-β-D-4C1-glucopyranosyl ester (9), was isolated from the leaves of Bauhinia variegata Linn. In addition, six flavonoid compounds along with two cinnamic acid derivatives were isolated and identified based on their chromatographic properties, and chemical and spectral data (ESI-high resolution-MSn, 1H NMR, 13C NMR, 1H-1H COSY, HSQC, and HMBC). Compound 9 was found to be nontoxic (LD50) and to have significant anti-inflammatory and antinociceptive activities. It also showed a slight antischistosomal activity.

Basic Chromium(III) Formate: Reaction of Chromiiim(III) Chloride with Formic Acid

1979 ◽  
Vol 34 (2) ◽  
pp. 160-162 ◽  
Author(s):  
R. C. Paul ◽  
P. Kapoor ◽  
. B. Baidya ◽  
R. Kapoor
Keyword(s):  
Formic Acid ◽  
Spectral Data ◽  
Magnetic Moment ◽  
Title Compound ◽  
Temperature Range ◽  
Infrared Spectral ◽  
Anhydrous Formic Acid

Abstract Chromium(III) Chloride, Basic Chromium(III) Formate, IR, Thermogravimetry, Magnetic Moment Chromium(III) chloride reacts with anhydrous formic acid to give basic chromium(III) formate [Cr3O(OOCH)6(H2O)2(HCOOH)](OOCH), HCOOH. Its reactions with bases (B) give compounds of the general composition [Cr30(C00CH)6(B)3](00CH). The title compound has been characterized by infrared spectral data, temperature range (266-110K) magnetic moment and thermogravimetry.

scholarly journals Some complexes of N-aryl furfural nitrones with Co (II), Ni (II), Cu (II), Zn (II) and Cd (II) chlorides

2016 ◽  
Vol 4 (1) ◽  
pp. 10
Author(s):  
Amer A. Taqa
Keyword(s):  
Spectral Data ◽  
General Formula ◽  
Elemental Analysis ◽  
13C Nmr ◽  
High Frequency ◽  
Metal Ion ◽  
Uv Spectroscopy ◽  
Active Atom ◽  
Tetrahedral Complexes

Some new metal(II) dichloride complexes with the ligands substituted nitrones of the general formula [ML2Cl2], where M= Co(II), Ni(II), Cu(II), Zn(II) and Cd(II), L=OCH=CHCH=C-CH=N(O)C6H4X (X=H,p-CH3,CH3O,CH3CO,F,Cl,and Br) have been prepared and characterized by elemental analysis, IR,1H,13C NMR and Vis/Uv spectroscopy. The IR spectral data showed that the nitrone ligands coordinated with the metal ion through the most active atom of the N-oxide to give square planner coordinate (Cu,Ni,) complexes and (Zn,Cd,Co) tetrahedral complexes. No correlation was observed between the N-O vibrations stretching high frequency ν (N-O) of the complexes and the Hammet (σ) constants.

A Chromone Based Fluorescent Probe for the Effective Detection of Aluminium Ion

2020 ◽  
Vol 20 (5) ◽  
pp. 2840-2846
Author(s):  
Hyorim Kim ◽  
Ramalingam Manivannan ◽  
Young-A Son
Keyword(s):  
Metal Ion ◽  
Color Change ◽  
Test Strip ◽  
Phenyl Hydrazine ◽  
Mass Spectral ◽  
H Nmr ◽  
Turn On ◽  
Molecular Charge ◽  
Intra Molecular Charge Transfer ◽  
Significant Interference

A new chromone moiety fused with phenyl hydrazine carboxamide as a binding site for metal ion was designed and synthesized as a colorimetric/fluorimetric probe for selective sensing of Al3+ ion. The absorption and fluorescence spectral results showed selective and sensitive recognition of Al3+ with no significant interference from other competitive metal ions. The addition of Al3+ to R brought a prompt color change from colorless to yellow and the turn-on fluorescence response with Al3+ among different cations was studied. The visible color change and turn-on fluorescence Al3+ ion with R was attributed to the intra molecular charge transfer transition. The plausible binding nature of the receptor with Al3+ has also been anticipated by the results of 1H NMR and mass spectral analysis. For the practical effectiveness, test strip prepared using probe R was successfully applied to monitor the presence of Al3+ ion in aqueous medium.

Notizen: Umsetzung von Tris-[dimethylaminino]-arsin mit Arsinigsäurediolestern, eine ungewöhnliche Arsolansynthese / Reaction of Tris-[dimethylamino]-arsine with Arsinous Acid Diolesters, an Unusual Synthesis of Arsolanes

1976 ◽  
Vol 31 (2) ◽  
pp. 190-193 ◽  
Author(s):  
Werner J. Rühl ◽  
Friedhelm Kober
Keyword(s):  
Reaction Mechanism ◽  
Spectral Data ◽  
H Nmr

The reaction of tris-[dimethylamino]-arsine As(NMe2)3 with arsinous acid diolesters HO—RO—AsMe2 leads to the formation of the arsolanes RO2AsY (Y = NMe2, OROAsMe2) and the arsines Me2AsX (X = NMe2, OROAsMe2). The reaction mechanism is discussed; IR and 1H NMR spectral data are presented.

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