Synthesis and Characterization of Cu(II) and Mono-and Dinuclear Pb(II) Complexes Derived from 3,5-Diacetyl-1,2,4-triazole

1994 ◽  
Vol 49 (5) ◽  
pp. 665-671 ◽  
Author(s):  
P. Souza ◽  
A. I. Matesanz ◽  
A. Arquero ◽  
V. Fernandez

Template 1:1 condensation of 3,5-diacetyl-1,2,4-triazole with thiocarbohydrazide or car- bohydrazide in the presence of 1 equivalent of Pb(SCN)2 produces mononuclear [2 + 1] com­plexes 1 and 3. The analogous reaction with thiosemicarbazide and semicarbazide produces the dinuclear [1+2] complex 2 and the mononuclear metal free 4. The carbohydrazide deriva­tive 3 reacts with the carbohydrazide or the 1,3-diaminopropane to yield the macrocyclic dinuclear complexes 5 and 6. Direct reaction of 3,5-diacetyl-1,2,4-triazole with thiocarbohydrazide. carbohydrazide, thiosemicarbazide and semicarbazide leads to open [1+1] ligands L1, L2, L3, L4, and closed [1+1] ligands (mesocyclic ligands) L5 and L6 were prepared by addition of 1 equivalent of LiOH to the reaction mixture. The reaction of open and mesocyclic [1+1] ligands with copper(II) salts gives [CuLX2] and [Cu2+L2-] complexes. All these compounds have been characterized by 1H NMR, IR, electronic and mass spectra and by analytical data.

1985 ◽  
Vol 63 (9) ◽  
pp. 2550-2554 ◽  
Author(s):  
Sophia Nussbaum ◽  
Alan Storr

The complexes [Me2Mpz2]Pt(Me)L (where L = CO, Ph3P, or PhC≡CPh for M = Ga; L = PhC≡CPh for M = B) have been synthesized by the direct reaction of the ligands Na[Me2Mpz2] with Pt(Me)Cl(COD) followed by the addition of ligand L. The complexes have been shown to be fluxional in solution by variable temperature 1H nmr methods.


2001 ◽  
Vol 05 (04) ◽  
pp. 367-375 ◽  
Author(s):  
S. ZEKİ YILDIZ ◽  
HALTİ KANTEKİN ◽  
YAŞAR GÖK

New metal-free 5 and metallophthalocyanines 6-11( M = Cu , Ni , Co , Pb , Zn ) fused in peripheral positions with four 24-membered tetraoxatetraaza macrocycles were prepared by cyclotetramerization of 24,25-dicyano-4,10,13,17-tetra(toluene-p-sulfonyl)-1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19,20,21,22-didicontinehydrobenzo[y][3,9,12,18]tetraaza[1,7,16,22]tetraoxatetradicontine in the presence of the corresponding metal salt or a strong organic base. While the N-tosylated derivatives of the phthalocyanines are soluble in common organic solvents, the detosylated derivative of copper phthalocyaninate is soluble in water. The aggregation properties of the phthalocyanines were also investigated as a function of concentration, solvent and oxidative medium. The new compounds are characterized by a combination of elemental analysis and 1 H NMR, 13 C NMR, IR, UV-vis and MS spectral data.


2002 ◽  
Vol 06 (07) ◽  
pp. 489-493 ◽  
Author(s):  
Gülay Gümüş ◽  
Vefa Ahsen

Metal-free- and metallophthalocyanines ( M = Ni , Zn and Co ) carrying four di-n-hexylamino and four chloro groups in peripheral positions have been synthesized from the corresponding dichlorophthalonitrile derivative in the presence of the anhydrous metal salts [ NiCl 2, Zn ( O 2 CMe )2, CoCl 2] or a strong organic base. The new compounds have been characterized by elemental analyses, IR, NMR and electronic spectroscopy and mass spectra.


2001 ◽  
Vol 05 (10) ◽  
pp. 717-720 ◽  
Author(s):  
M. S. AǦIRTAŞ ◽  
Ö. BEKAROǦLU

The synthesis of new metal-free and zinc(II), cobalt(II) phthalocyanines substituted with four 4-(2-N'-cyanoethyl)aminoethylsulfanyl groups is described. The new compounds have been characterized by elemental analysis and IR, 1 H NMR and UV-vis spectroscopy.


2011 ◽  
Vol 282-283 ◽  
pp. 116-119
Author(s):  
Zhi Yong Yang ◽  
Jin Shui Yao ◽  
Rui Bao Guo

A novel chiral poly(amide imide) containing L-alanine was synthesized by direct polycondensation reaction of newly synthesized N,N’-(4,4’-diphthaloyl)-bis-L-alanine diacid with 4,4’-diaminodiphenyl ether in a medium consisting of N-methyl-2-pyrrolidone (NMP), triphenylphosphite (TPP), calcium chloride (CaCl2), and pyridine. The new chiral diimide-diacid monomer was synthesized by direct reaction of 3,3’-4,4’-Biphenyl tetracarboxylic acid dianhydride with L-alanine in acetic acid under refluxing conditions. The resulting compounds were obtained in quantitative yields and high purity. The synthetic diacid monomer was characterized by elemental analysis,1H-NMR spectroscopy, FT-IR techniques and specific rotation, the obtained polymer was characterized by FTIR techniques, specific rotation and solubility testing.


2019 ◽  
Vol 17 (3) ◽  
pp. 541-554
Author(s):  
Neeranuth Intakaew ◽  
Puracheth Rithchumpon ◽  
Chanatkran Prommin ◽  
Saranphong Yimklan ◽  
Nawee Kungwan ◽  
...  

New chiral derivatizing agents and the effect of aromatic rings were investigated for absolute configuration of chiral alcohols via1H-NMR.


e-Polymers ◽  
2021 ◽  
Vol 21 (1) ◽  
pp. 491-499
Author(s):  
Fukai Yang ◽  
Hao Yu ◽  
Yuyuan Deng ◽  
Xinyu Xu

Abstract In this article, five kinds of soybean oil-based polyols (polyol-E, polyol-P, polyol-I, polyol-B, and polyol-M) were prepared by ring-opening the epoxy groups in epoxidized soybean oil (ESO) with ethyl alcohol, 1-pentanol, isoamyl alcohol, p-tert-butylphenol, and 4-methoxyphenol in the presence of tetrafluoroboric acid as the catalyst. The SOPs were characterized by FTIR, 1H NMR, GPC, viscosity, and hydroxyl numbers. Compared with ESO, the retention time of SOPs is shortened, indicating that the molecular weight of SOPs is increased. The structure of different monomers can significantly affect the hydroxyl numbers of SOPs. Due to the large steric hindrance of isoamyl alcohol, p-hydroxyanisole, and p-tert-butylphenol, SOPs prepared by these three monomers often undergo further dehydration to ether reactions, which consumes the hydroxyl of polyols, thus forming dimers and multimers; therefore, the hydroxyl numbers are much lower than polyol-E and polyol-P. The viscosity of polyol-E and polyol-P is much lower than that of polyol-I, polyol-B, and polyol-M. A longer distance between the molecules and the smaller intermolecular force makes the SOPs dehydrate to ether again. This generates dimer or polymers and makes the viscosity of these SOPs larger, and the molecular weight greatly increases.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Evelyn Carolina Martínez Ceballos ◽  
Ricardo Vera Graziano ◽  
Gonzalo Martínez Barrera ◽  
Oscar Olea Mejía

Poly(dichlorophosphazene) was prepared by melt ring-opening polymerization of the hexachlorocyclotriphosphazene. Poly[bis(2-hydroxyethyl-methacrylate)-phosphazene] and poly[(2-hydroxyethyl-methacrylate)-graft-poly(lactic-acid)-phosphazene] were obtained by nucleophilic condensation reactions at different concentrations of the substituents. The properties of the synthesized copolymers were assessed by FTIR,1H-NMR and31P-NMR, thermal analysis (DSC-TGA), and electron microscopy (SEM). The copolymers have a block structure and show twoTg's below room temperature. They are stable up to a temperature of 100°C. The type of the substituents attached to the PZ backbone determines the morphology of the polymers.


1993 ◽  
Vol 48 (12) ◽  
pp. 1781-1783 ◽  
Author(s):  
Abdel-Fattah Shihada

(Me3Sn)3PO3S has been prepared from the reaction of Me3SnCl with Na3PO3S • 12 H2O under cooling in aqueous medium. Its IR and Raman spectra are found to be consistent with a polymeric structure with tetra- and penta-coordinated tin atoms. The 31P NMR and mass spectra of (Me3Sn)3PO3S are reported and discussed.


2015 ◽  
Vol 19 (01-03) ◽  
pp. 335-343 ◽  
Author(s):  
Vicente M. Blas-Ferrando ◽  
Javier Ortiz ◽  
Fernando Fernández-Lázaro ◽  
Ángela Sastre-Santos

This work reports on the synthesis and characterization of a new gold nanoparticle-zinc phthalocyanine system, AuNP - S (t Bu )3 ZnPc , prepared by a ligand exchange reaction of tetraoctylammonium bromide with a novel unsymmetrically substituted zinc phthalocyanine which contains one thioester group in the peripheral position [ AcS (t Bu )3 ZnPc ]. The AuNP - S (t Bu )3 ZnPc hybrid was characterized using UV-vis and 1 H NMR spectroscopies. Transmission electron microscopy allowed the estimation of the size, which was calculated to be ~5 nm. AuNPs - S (t Bu )3 ZnPc conjugate showed much lower fluorescence quantum yield values than the AcS (t Bu )3 ZnPc demonstrating either an energy or electron transfer from the ZnPc to the AuNP . The AuNP - S (t Bu )3 ZnPc hybrid has been anchored to a TiO 2 semiconducting layer using lipoic acid. A solid configuration of TiO 2-lipoic acid- AuNP - S (t Bu )3 ZnPc has been prepared by anchoring lipoic acid to the TiO 2 ( TiO 2-LA) and introducing later the TiO 2-LA with free thiol groups in a toluene solution of AuNP - S (t Bu )3 ZnPc . We have also observed by UV-vis and fluorescence measurements the importance of the ZnPc in avoiding AuNP aggregation on the TiO 2 surface.


Sign in / Sign up

Export Citation Format

Share Document