New Polymer Synthesis 99. Hyperbranched Poly(Ester-Imide)S Derived from 4,5-Dichlorophthalic Acid

1998 ◽  
Vol 10 (3) ◽  
pp. 217-229 ◽  
Author(s):  
Hans R Kricheldorf ◽  
Oliver Bolender ◽  
Thomas Wollheim
Keyword(s):  
Nmr Spectra ◽  
Variable Degree ◽  
Carboxylic Group ◽  
Degree Of Branching ◽  
Glass Transition Temperatures ◽  
Oh Groups ◽  
H Nmr ◽  
Hyperbranched Poly ◽  
Elemental Analyses ◽  
Phenolic Oh Groups

A new trifunctional monomer was prepared from ethyl-4-(4,5-dichlorophthalimido) benzoate and 4-mercaptophenol. The phenolic OH groups were acetylated, and the carboxylic group was silylated to reduce the melting temperature. A successful homopolycondensation yielding a completely soluble hyperbranched poly(ester-imide) was only obtained when the silylated monomer was used. This branching monomer was polycondensed with a difunctional imide monomer to yield co(polyester-imide)s having a variable degree of branching. Furthermore, copolycondensations with 3-acetoxybenzoic acid or 3,5-bisacetoxybenzoic acid (and their trimethylsilyl esters) were studied. The composition of the resulting copolyesters were checked by elemental analyses and 1H NMR spectra. The glass transition temperatures ( T g s) showed a systematic variation between the values of the parent homopolyesters.

119Sn, 13C and 1H NMR Spectra of Tris(1-butyl)stannyl D-Glucuronate

1997 ◽  
Vol 62 (8) ◽  
pp. 1169-1176 ◽  
Author(s):  
Antonín Lyčka ◽  
Jaroslav Holeček ◽  
David Micák
Keyword(s):  
Chemical Shift ◽  
Carbonyl Group ◽  
1H Nmr ◽  
Equatorial Plane ◽  
Title Compound ◽  
Nmr Spectra ◽  
Hydroxyl Groups ◽  
Carboxylic Group ◽  
H Nmr ◽  
Oxygen Atoms

The 119Sn, 13C and 1H NMR spectra of tris(1-butyl)stannyl D-glucuronate have been measured in hexadeuteriodimethyl sulfoxide, tetradeuteriomethanol and deuteriochloroform. The chemical shift values have been assigned unambiguously with the help of H,H-COSY, TOCSY, H,C-COSY and 1H-13C HMQC-RELAY. From the analysis of parameters of 119Sn, 13C and 1H NMR spectra of the title compound and their comparison with the corresponding spectra of tris(1-butyl)stannyl acetate and other carboxylates it follows that in solutions of non-coordinating solvents (deuteriochloroform) the title compound is present in the form of more or less isolated individual molecules with pseudotetrahedral environment around the central tin atom and with monodentately bound carboxylic group. The interaction of tin atom with oxygen atoms of carbonyl group and hydroxyl groups of the saccharide residue - if they are present at all - are very weak. In solutions in coordinating solvents (hexadeuteriodimethyl sulfoxide or tetradeuteriomethanol), the title compound forms complexes with one molecule of the solvent. Particles of these complexes have a shape of trigonal bipyramid with the 1-butyl substituents in equatorial plane and the oxygen atoms of monodentate carboxylic group and coordinating solvent in axial positions.

scholarly journals Metallkomplexe mit Tetrapyrrol-Liganden, XXXVIII [1]. Zur Kenntnis der Alkyl- und Arylimidovanadium(IV)-Porphyrine / Metal Complexes with Tetrapyrrole Ligands, XXXVIII [1]. On the Knowledge of Alkyl- and Arylimidovanadium(IV) Porphyrins

1985 ◽  
Vol 40 (10) ◽  
pp. 1362-1370 ◽  
Author(s):  
Johann W. Buchler ◽  
Stefan Pfeifer
Keyword(s):  
Mass Spectra ◽  
Nmr Spectra ◽  
Primary Amines ◽  
Reactive Intermediate ◽  
H Nmr ◽  
Vanadyl Complex ◽  
Elemental Analyses ◽  
Paramagnetic Metal ◽  
Paramagnetic Complexes ◽  
Proton Resonances

A series of novel alkyl or aryiimidovanadium(IV) 5,10,15,20-tetra(p-tolyl)porphyrinates, VNR(TTP) (4a-4g), is described. They are obtained from the vanadyl complex, VO(TTP) (2a) via the reactive intermediate VCl2(TTP) (3b) which undergoes aminolysis with the respective primary amines RNH2 (R = tBu, Ph, pTol, pClPh, pAnis, pBiph, ptBuPh)**. The formulae are proved by elemental analyses and mass spectra. The paramagnetic complexes are stable to water and may thus be purified by chromatography but are hydrolyzed to give 2 a on treatment with acetic acid. The UV/VIS and 1H NMR spectra of 4a-4g are of the same type as 2a, but the former are slightly hypsochromically shifted, and the latter do not show the proton resonances of the organylimide ligands due to the proximity of the paramagnetic metal center.

Synthesis and Characterization of a Novel Hyperbranched Poly(Diethynylbenzene-Silane)

2012 ◽  
Vol 560-561 ◽  
pp. 174-178
Author(s):  
Yan Zou ◽  
Hui Min Qi ◽  
Mei Ling Xu ◽  
Fa Rong Huang ◽  
Lei Du
Keyword(s):  
Thermal Stability ◽  
Grignard Reagent ◽  
Synthesis And Characterization ◽  
Polycondensation Reaction ◽  
Degree Of Branching ◽  
H Nmr ◽  
Hyperbranched Poly ◽  
Ft Ir ◽  
Thermal Stability Of

Hyperbranched poly(diethynylbenzene-silane) (hb-PDEBS) was synthesized through polycondensation reaction of diethynylbenzene Grignard reagent (A2) and trichlorosilane (B3), and its structure was characterized by FT-IR, 1H-NMR, GPC and Elemental Analysis. The degree of branching of hb-PDEBS was defined by 29Si-NMR and calculated to be about 0.68. The curing behavior of hb-PDEBS was investigated by DSC. Thermal stability of cured hb-PDEBS was examined by TGA, and its residue at 1000°C under nitrogen was 80.6%. Hb-PDEBS displayed a strong absorption due to π-π* transition and exhibited the most intensity structured emission with a maximum around 500 nm.

Reaction of Ester Ethoxycarbonylhydrazones with Aliphatic Diamines

1995 ◽  
Vol 60 (5) ◽  
pp. 903-909 ◽  
Author(s):  
Aykut A. Ikizler ◽  
Kemal Sancak
Keyword(s):  
Nmr Spectra ◽  
H Nmr ◽  
Elemental Analyses ◽  
Aliphatic Diamines

Reaction of esters of (N-ethoxycarbonyl)alkanehydrazonic acids with aliphatic diamines were prepared α,ω-bis(3-alkyl-4,5-dihydro-1H -1,2,4-triazol-5- one-4-yl)alkanes. All compounds were characterized by elemental analyses, IR and 1H NMR spectra.

scholarly journals Synthesis and Antimicrobial Screening of Novel 4-Substituted Phenyl-5-[1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-yl]-2H-1,2,4-triazole-3-thiones

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Namratha Bhandari ◽  
Santosh L. Gaonkar
Keyword(s):  
Convenient Method ◽  
Nmr Spectra ◽  
Spectral Studies ◽  
Antimicrobial Screening ◽  
Antifungal Activities ◽  
H Nmr ◽  
Antibacterial And Antifungal Activities ◽  
Elemental Analyses ◽  
Antibacterial And Antifungal ◽  
C Nmr

The paper describes a convenient method for the preparation of 4-substituted phenyl-5-[1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-yl]-2H-1,2,4-triazole-3-thiones. The structures of the synthesized compounds are established by the results of LCMS, 1H NMR, 13C NMR, and IR and elemental analyses. The mercaptotriazoles are indicated to be in thione form by 1H NMR spectra. All the synthesized compounds have been screened for antibacterial and antifungal activities. Compounds 12d and 12h exhibit encouraging results, while the remaining compounds show moderate activities. On the basis of spectral studies, formation of 2-amino-1,3,4-thiadiazoles from the isobenzofuran acyl thiosemicarbazides 11(a–h) is ruled out.

scholarly journals Structural characterization and DNA-binding properties of Sm(III) complex with ofloxacin using spectroscopic methods

2009 ◽  
Vol 23 (2) ◽  
pp. 103-111 ◽  
Author(s):  
Changyun Chen ◽  
Kai Chen ◽  
Qi Long ◽  
Meihua Ma ◽  
Fei Ding
Keyword(s):  
Binding Sites ◽  
Nmr Spectra ◽  
Uv Spectroscopy ◽  
Binding Constants ◽  
Binding Properties ◽  
H Nmr ◽  
Elemental Analyses ◽  
Displacement Experiments ◽  
Ct Dna ◽  
Dna Binding Properties

A novel complex Sm(III) complex with ofloxacin was synthesized and characterized on the basis of elemental analyses, molar conductivities, IR spectra, thermal analysis (TG-DSC),1H-NMR spectra. Then, spectrometric titration, ethdium bromide displacement experiments by UV spectroscopy, ionic influence, viscosity measurements and Circular Dichroism (CD) spectroscopic measurements were conducted to characterize the interaction between the complex and CT-DNA. Results obtained indicate that the complex bound with CT-DNA via an intercalation mechanism. The binding constants and binding sites number of the Sm(III) complex with CT-DNA were 1.80×105l·mol−1and 1, respectively.

One-pot approach to synthesize hyperbranched poly(thiol–ether amine) (hPtEA) through sequential “thiol–ene” and “epoxy–amine” click reactions

2015 ◽  
Vol 6 (39) ◽  
pp. 6946-6954 ◽  
Author(s):  
Jing Yu ◽  
Zhilong Su ◽  
Hongjie Xu ◽  
Xiaodong Ma ◽  
Jie Yin ◽  
...  
Keyword(s):  
Nmr Spectra ◽  
One Pot ◽  
Click Reactions ◽  
H Nmr ◽  
Epoxy Amine ◽  
Hyperbranched Poly

We demonstrated a one-pot approach to synthesize hyperbranched poly(thiol–ether amine) (hPtEA) through sequential “thiol–ene” and “epoxy–amine” click reactions, both of which were well traced using in situ1H-NMR spectra.

Synthesis of new phthalocyanines substituted with four 1H-benzoimidazol-2-ylsulfanyl and 2-(1H-benzo[d]imidazol-2-ylthioetoxy) groups

2006 ◽  
Vol 10 (02) ◽  
pp. 117-121 ◽  
Author(s):  
M. Salih Ağırtaş ◽  
Ümit Yıldıko ◽  
Ayfer Yılan
Keyword(s):  
Nmr Spectra ◽  
H Nmr ◽  
Elemental Analyses ◽  
Uv Visible

The synthesis of new two phthalonitrile derivatives is described. Using these starting materials, metallophthalocyanines substituted with four 1 H -benzoimidazol-2-ylsulfanyl and 2-(1 H -benzo[d]imidazol-2-ylthioetoxy) have been synthesized, respectively. The newly synthesized compounds have been characterized by elemental analyses, UV-visible, IR and 1 H NMR spectra.

1: 13- und 1: 14-Heteropolyvanadate des Phosphors(V) / 1:13- and 1:14- Heteropolyvanadates of Phosphorus(V)

1976 ◽  
Vol 31 (12) ◽  
pp. 1585-1591 ◽  
Author(s):  
Fritz Preuss ◽  
Heinrich Schug
Keyword(s):  
Molecular Weight ◽  
Nmr Spectra ◽  
Soluble Salts ◽  
Oh Groups ◽  
H Nmr ◽  
Stable Species ◽  
Wide Range ◽  
Wide Line

Deep red heteropolyvanadates of phosphorus(V) n M2O:P2O5: 13 V2O5 · aq (n = 3, 5, 6; M = Na, K, Rb, Cs, NH4) and n M2O: P2O5: 14 V2O5 · aq (n = 4, 7; M = K, Rb, Cs, NH4, (n-C4H9)4N) were prepared. Recrystallization of 1: 13- and 1: 14-heteropolyvanadates and determination of molecular weight by ultracentrifuge technique in solutions from V2O5 and NaH2PO4 indicate 1: 14-heteropolyvanadate ions to be stable species over a wide range of pH, while 1: 13-heteropolyvanadate ions are only stabilized in higher acidified solutions containing H2PO4- or as slightly soluble salts. Wide line 1H NMR spectra are interpreted in terms of OH groups and H2O of cristallization, the isolated heteropolyvanadates of both series consisting of protonated anions; the basicity of heteropolyvanadic acids of phosphorus(V) is unknown.

Synthesis of Substituted Furo[2',3':4,5]pyrrolo[1,2-d][1,2,4]triazolo[3,4-f][1,2,4]triazines

1995 ◽  
Vol 60 (4) ◽  
pp. 709-714 ◽  
Author(s):  
Vladimír Bobošík ◽  
Alžbeta Krutošíková ◽  
Miloslava Dandárová
Keyword(s):  
Nmr Spectra ◽  
H Nmr ◽  
Elemental Analyses

The title compounds were prepareed by reaction of 1,2-dihydrofuro[2',3':4,5]pyrolo[1,2-d][1,2,4]-1-hydrazones by cyclization with triethyl orthoformiate or triethyl orthoacetate. All compounds were characterized by elemental analyses, UV and 1H NMR spectra.

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