Synthesis and characterization of new metal-free and metal phthalocyanines with peripheral N'-2-(cyanoethyl)-aminoethylsulfanyl substituents

2001 ◽  
Vol 05 (10) ◽  
pp. 717-720 ◽  
Author(s):  
M. S. AǦIRTAŞ ◽  
Ö. BEKAROǦLU
Keyword(s):  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
Metal Phthalocyanines ◽  
Metal Free ◽  
H Nmr ◽  
Vis Spectroscopy ◽  
New Compounds

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.

Synthesis and characterization of novel metal-free and metallophthalocyanines peripherally fused to four 24-membered tetraoxatetraaza macrocycles

2001 ◽  
Vol 05 (04) ◽  
pp. 367-375 ◽  
Author(s):  
S. ZEKİ YILDIZ ◽  
HALTİ KANTEKİN ◽  
YAŞAR GÖK
Keyword(s):  
Elemental Analysis ◽  
Metal Salt ◽  
Synthesis And Characterization ◽  
Organic Base ◽  
Metal Free ◽  
H Nmr ◽  
New Compounds ◽  
Derivatives Of ◽  
C Nmr

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.

Titanocene derivatives of purine and adenine. Synthesis and characterization of reaction products with (η5-C5H5)2Ti(CO)2, (η5-C5H5)2TiCl, and (η5-C5H5)2TiCl2

1986 ◽  
Vol 64 (4) ◽  
pp. 751-759 ◽  
Author(s):  
Daniel Cozak ◽  
Abdelhakim Mardhy ◽  
André Morneau
Keyword(s):  
Carbon Monoxide ◽  
Metal Complex ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
Reaction Products ◽  
First Order ◽  
H Nmr ◽  
New Compounds ◽  
Derivatives Of

The reaction of CpTi(CO)2 (1), Cp2TiCl (2), and Cp2TiCl2 (3) (Cp = η5-C5H5) with purine (PuH) and adenine (AdH) in organic solvents is described. The compound 1 reacts with both molecules in an oxidative fashion giving Cp2Ti(C5H3N4)(C5H4N4) (4) and (Cp2Ti)2(C5H3N5) (5) with concomitant liberation of molecular carbon monoxide and hydrogen (4:1) following a first order rate law in metal complex. The compound 2 forms an adduct compound Cp2TiCl(C5H4N4) (6) with PuH. Monosubstituted derivatives Cp2TiCl(C5H3N4) (7) and Cp2TiCl(C5H4N5) (8) are formed from the reaction of the deprotonated bases with 3. In addition to the usual elemental analysis, the characteristic ir, 1H nmr, epr, and ms results are given for the new compounds.

Synthesis and spectral characterization of bis(β-diketonato)zirconium(IV) and -hafnium(IV) phthalocyaninates

2002 ◽  
Vol 06 (02) ◽  
pp. 114-121 ◽  
Author(s):  
L. A. Tomachynski ◽  
V. Ya. Chernii ◽  
S. V. Volkov
Keyword(s):  
Organic Solvents ◽  
Elemental Analysis ◽  
Central Atom ◽  
Spectral Characterization ◽  
H Nmr ◽  
Vis Spectroscopy ◽  
Cl Atoms

The reaction of PcMCl 2 ( M = Zr , Hf ) with β-diketones is reported. 1 H NMR and elemental analysis suggest the substitution of two Cl atoms for two β-diketone fragments takes place as a result of this reaction and the complexes PcM(β-dik)2 are formed. All obtained complexes are stable and highly soluble in most organic solvents. The data from 1 H and 19 F NMR, and UV-vis spectroscopy suggest the coordination of two β-diketone ligands in a cis geometry about the central atom of the macrocycle. It was shown bis(β-diketonato)zirconium(IV) and hafnium(IV) phthalocyanines containing β-diketones with donor or acceptor groups or with bulky substituents can be obtained.

Synthesis and characterization of N-glucosylated dithiadiazepine derivatives through carbon-sulfur bond formation

2015 ◽  
Vol 21 (5) ◽  
pp. 269-272 ◽  
Author(s):  
Snehal A. Chavan ◽  
Avinash G. Ulhe ◽  
Baliram N. Berad
Keyword(s):  
Bond Formation ◽  
Synthesis And Characterization ◽  
Mass Spectral ◽  
H Nmr ◽  
Chemical Structures ◽  
Elemental Analyses ◽  
New Compounds ◽  
Sulfur Bond ◽  
C Nmr

AbstractNew 4,7-bis(arylamino)-2-tetra-O-acetyl-β-d-glucopyranosylimino-1,3,5,6-dithiadiazepines were synthesized via reaction of N-tetra-O-acetyl-β-d-glucopyranosyl isocyanodichloride with 1,6-diaryl-2,5-dithio-bis-ureas without using any catalyst. Thus, the synthesis of 7-membered heterocycles containing two sulfur and two nitrogen atoms through carbon-sulfur bond formation was explored. The chemical structures of these new compounds were elucidated by IR, 1H NMR, 13C NMR, mass spectral, and elemental analyses.

Synthesis and characterization of O- and S-bridged perfluoroalkylated metal-free and zinc phthalocyanines

2013 ◽  
Vol 17 (06n07) ◽  
pp. 555-563 ◽  
Author(s):  
İlke Gürol ◽  
Gülay Gümüş ◽  
Emel Musluoğlu ◽  
Yadigar Arslan ◽  
Vefa Ahsen
Keyword(s):  
Nucleophilic Substitution ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
Polar Solvents ◽  
Metal Free ◽  
Zinc Phthalocyanines ◽  
Ft Ir

The synthesis of tetra and octa perfluoroalkyl substituted zinc and metal free phthalocyanines ( ZnPc and H 2 Pc ) are reported. The compounds 1–5 have been prepared by nucleophilic substitution of 4-nitrophthalonitrile with 1H,1H,2H,2H-perfluorooctanethiol, 1H,1H,2H,2H-perfluorodecan-1-ol, 1H,1H-perfluorodecan-1-ol, 1H,1H-perfluorotetradecan-1-ol and 1H,1H-perfluoro-3,6,9-trioxatridecan-1-ol, respectively. The compounds 6–8 have been prepared by the reaction of 1H,1H,2H,2H-perfluorodecan-1-ol, 1H,1H-perfluorodecan-1-ol and 1H,1H-perfluoro-3,6,9-trioxatridecan-1-ol with 4,5-dichlororphthalonitrile, respectively. The compound 9 with thia-bridge has been synthesized from 4,5-dichlororphthalonitrile. Zinc and metal free phthalocyanines were obtained from the corresponding phthalonitrile derivatives. All compounds were characterized by using mass, 1 H , 19 F NMR, UV-vis and FT-IR as well as elemental analysis. Tetra substituted Zn ( II ) phthalocyanines are slightly soluble only in THF (Compound 4a and 7a are insoluble) but metal free phthalocyanines are not soluble. Octa substituted Zn ( II ) and metal free phthalocyanine are soluble in polar solvents such as THF and DMSO.

scholarly journals Synthesis, structures and reduction chemistry of monophthalocyanine scandium hydroxides

2019 ◽  
Vol 23 (11n12) ◽  
pp. 1592-1602 ◽  
Author(s):  
Yumeela Ganga-Sah ◽  
Elahe Tajbakhsh ◽  
Rachel H. Platel ◽  
Wen Zhou ◽  
Daniel B. Leznoff
Keyword(s):  
Alkali Metal ◽  
Dihedral Angles ◽  
Ambient Atmosphere ◽  
Metal Alkoxides ◽  
Metal Free ◽  
H Nmr ◽  
Vis Spectroscopy ◽  
Hydrolysis Of ◽  
Direct Hydrolysis

The preparation and structural characterization of a pair of scandium(III) phthalocyanine hydroxide complexes were achieved by reaction of PcScCl with alkali metal alkoxides, likely via hydrolysis of soluble PcSc-alkoxide intermediates. A Sc[Formula: see text]Li[Formula: see text]-OH)[Formula: see text] cubane supported by two distorted Pc rings of the form (PcSc)[Formula: see text]-OH)[Formula: see text]Li[Formula: see text](THF)(DME) was isolated from the reaction of PcScCl with LiO[Formula: see text]Pr, while a simpler alkali-metal-free [Pc[Formula: see text]Sc[Formula: see text]-OH)[Formula: see text](THF)] was obtained from addition of NaO[Formula: see text]Bu; both structures are reminiscent of bent metallocenes, with dihedral angles between the two Pc rings of 50.8 and 37.7[Formula: see text]respectively. A soluble PcScOH material can also be obtained directly via hydrolysis of insoluble PcScCl in approximately 95:5 THF:water. Reduction of the Pc ring of PcScCl using KC[Formula: see text] is reversible and generates Pc[Formula: see text] and Pc[Formula: see text]-containing materials that were characterized via UV-vis spectroscopy and, where appropriate EPR and [Formula: see text]H NMR spectroscopy; analogous reductions of the PcScOH-based species were irreversible. Exposure of the air-sensitive, reduced PcScCl-based species to ambient atmosphere generated PcScOH materials analogous to the direct hydrolysis route.

Synthesis and Characterization of a Three-dimensional Porous Compound: [Cu(H2O)6][{Cu(H2O)2}2{Cu(H2O)4H4W12O42}] · 12H2O

2008 ◽  
Vol 63 (2) ◽  
pp. 187-192 ◽  
Author(s):  
Chun-jing Zhang ◽  
Ya-guang Chen ◽  
Dong-mei Shi ◽  
Hai-jun Pang
Keyword(s):  
Aqueous Solution ◽  
Magnetic Susceptibility ◽  
Elemental Analysis ◽  
3D Structure ◽  
Three Dimensional ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy

A novel transition metal polyoxotungstate, [Cu(H2O)6][{Cu(H2O)2}2{Cu(H2O)4H4W12O42}] · 12H2O (1), has been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction, elemental analysis, IR and UV/vis spectroscopy, and TG analysis. The paradodecatungstate anions [H2W12O42]10− are linked by CuO6 octahedra, forming a three-dimensional (3D) structure. The magnetic susceptibility of compound 1 in the temperature range 2 - 300 K shows the presence of antiferromagnetic interactions within the uniform Cu2・ ・ ・Cu3 chains

Water-soluble manganese phthalocyanines

2013 ◽  
Vol 17 (08n09) ◽  
pp. 881-888 ◽  
Author(s):  
Olga Dolotova ◽  
Olga Yuzhakova ◽  
Ludmila Solovyova ◽  
Ekaterina Shevchenko ◽  
Vladimir Negrimovsky ◽  
...  
Keyword(s):  
Coordination Chemistry ◽  
Aqueous Solutions ◽  
Elemental Analysis ◽  
High Purity ◽  
Water Soluble ◽  
Metal Free ◽  
Organic Bases ◽  
New Findings ◽  
Vis Spectroscopy ◽  
New Compounds

Three new substituted manganese phthalocyanines (PcMns), wich are water-soluble, have been synthesized with good yields (70–80%) and high purity. Pyridiniummethyl- and cholinylsubstituted phthalocyanines have been obtained from the chloromethylsubstituted PcMns , while octacarboxysubstituted complex has been synthesized from metal-free octacarboxyphthalocyanine tetraanhydride. Compounds were characterized by elemental analysis and mass, IR and UV-vis spectroscopy. In general, coordination chemistry of the compounds studied is similar to this one of liposoluble PcMns but some new findings have been obtained. Three coordination forms — PcMn ( II ), PcMn ( III ) X ( X = Cl -, OAc -, …) and [ LPcMn ( III )]2 O ( L = Py , Et 3 N , …) have been obtained for all the new compounds. The equilibrium between three electronic isomers — Pc+• Mn ( I ) × L , PcMn ( II ) × nL , (n = 1, 2) and Pc-• Mn ( III ) × 2 L has been observed in PcMn aqueous solutions upon the addition of organic bases L ( Py , Et 3 N , …).

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
Keyword(s):  
Mass Spectra ◽  
Analytical Data ◽  
Synthesis And Characterization ◽  
Dinuclear Complexes ◽  
Direct Reaction ◽  
Analogous Reaction ◽  
Metal Free ◽  
H Nmr

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.

The first synthesis and characterization of new metal-free and metallophthalocyanine containing 33-membered crown ether moieties

2013 ◽  
Vol 17 (06n07) ◽  
pp. 473-479 ◽  
Author(s):  
Fatma Akkuş ◽  
Nilgün Kabay ◽  
Yaşar Gök
Keyword(s):  
Crown Ether ◽  
Spectral Data ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
The Novel ◽  
Metal Free ◽  
C Nmr

The synthesis and characterization of novel metal-free and metallophthalocyanines, fused symmetrically in non-peripheral positions with four octaoxamacrocycle has been synthesized by cyclotetramerization of the 2,5,8,11,14,20,23,26,29,32-decaoxatricyclo [31.2.2.115,19]octatriconta-1(36),15,17,19(38),33(37),34-hexaene-34,35-dicarbonitrile (5) which was prepared by the reaction of 3,6-bis[2-(2-{2-[2-(toluene-4-sulphonyl)-ethoxy]-ethoxy}-ethoxy)-ethoxy]-phthalonitrile (3) and 1,3-dihydroxybenzene (4). The novel compounds were characterized by using elemental analysis, 1 H , 13 C NMR, IR, UV-vis and MS spectral data.

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