scholarly journals Fluorinated maleimide-substituted porphyrins and chlorins: synthesis and characterization

2019 ◽  
Vol 15 ◽  
pp. 2704-2709
Author(s):  
Valentina A Ol’shevskaya ◽  
Elena G Kononova ◽  
Andrei V Zaitsev
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Maleic Anhydride ◽  
Click Reaction ◽  
Synthesis And Characterization ◽  
H Nmr

Maleimide-containing fluorinated porphyrins and chlorins were prepared based on the reaction of Zn(II) or Ni(II) complexes of 5,10,15,20-tetrakis(4-amino-2,3,5,6-tetrafluorophenyl)porphyrin and chlorin with maleic anhydride. Porphyrin maleimide derivatives were also prepared by the reaction of 5,10,15,20-tetrakis(4-azido-2,3,5,6-tetrafluorophenyl)porphyrinato Zn(II) or Ni(II) with N-propargylmaleimide via the CuAAC click reaction to afford fluorinated porphyrin–triazole–maleimide conjugates. New maleimide derivatives were isolated in reasonable yields and identified by UV–vis, 1H NMR, 19F NMR spectroscopy and mass-spectrometry.

Chemie polyfunktioneller Liganden, 69 [1] Über drei Organo-Arsen-Käfigverbindungen mit Noradamantanstruktur / Chemistry of Polyfunctional Ligands, 69 [1] Three Organo-Arsenic Cage Compounds with Noradamantane Structure

1981 ◽  
Vol 36 (12) ◽  
pp. 1532-1537 ◽  
Author(s):  
Jochen Ellermann ◽  
Martin Lietz
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Cage Compounds ◽  
H Nmr ◽  
New Compounds

Abstract The reaction of l.l.l-tris(diiodarsinomethyl)ethane, CH3C(CH2Asl2)3 (1), with H2C(COOC2H5)2, H2C(COOCH3)2 and H2C(COC6H5)2 in presence of the auxiliary base (C2H5)3N gives the noradamantane structured compounds CH3C(CH2As)3E2 [E=C(COOC2H 5)2 (2), C(COOCH3)2 (3) and C(COC6H5)2 (4)].The new compounds have been characterized by mass spectrometry and infrared, Raman and 1H NMR spectroscopy.

New peripherally substituted lutetium mono and bis phthalocyanines: Synthesis and comparative photophysical and photochemical properties

2019 ◽  
Vol 23 (11n12) ◽  
pp. 1542-1550
Author(s):  
Nagihan Kocaağa ◽  
Öznur Dülger Kutlu ◽  
Ali Erdoğmuş
Keyword(s):  
Mass Spectrometry ◽  
Photodynamic Therapy ◽  
Singlet Oxygen ◽  
Photophysical Properties ◽  
Quantum Yields ◽  
Synthesis And Characterization ◽  
Type Ii ◽  
H Nmr ◽  
Photochemical Properties

In this study, the synthesis and characterization of mono-(phthalocyaninato) lutetium(III) (1-Cl and 1-F) [Lu[Formula: see text](AcO)(Pc)] (Pc [Formula: see text] phthalocyaninato, AcO [Formula: see text] acetate) and bis-(phthalocyaninato) lutetium(III) (2-Cl and 2-Br) [Lu[Formula: see text]Pc[Formula: see text]] bearing halogenated (F, Cl and Br) phenoxy–phenoxy groups are described and verified by IR, [Formula: see text]H-NMR, UV-vis and mass spectrometry. Photochemical and photophysical properties of 1-F, 1-Cl 2-Cl and 2-Br in DMSO are also presented. A comparison between photophysical and photochemical parameters of mono and bis derivatives showed that mono phthalocyanines are better photosensitizers than bis phthalocyanines. Photophysical and photochemical properties of phthalocyanines are very useful for photodynamic therapy applications. Singlet oxygen quantum yields [Formula: see text] give an indication of the potential of the complexes as photosensitizers in photodynamic therapy applications. The chloro, fluoro, bromo-phenoxy–phenoxy substituted mono-(phthalocyaninato) lutetium(III) complexes (1-Cl and 1-F) gave good singlet oxygen quantum yields (from 0.86 to 0.80) in DMSO. Thus, these complexes show potential as Type II photosensitizers for PDT of cancer.

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.

The Synthesis and Characterization of Nitrooxy- and Nitrosooxyborazine Compounds

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1241-1247
Author(s):  
Thomas M. Klapötke ◽  
Magdalena Rusan
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Vibrational Spectroscopy ◽  
Elemental Analysis ◽  
Experimental Results ◽  
Synthesis And Characterization ◽  
The Impact

Abstract B-Nitrosooxypentamethylborazine, B-nitrooxypentamethylborazine and B-trinitrooxy-N-trimethylborazine have been synthesized and characterized by 1H, 13C, 11B, and 14N NMR spectroscopy, mass spectrometry, vibrational spectroscopy and elemental analysis. The 11B NMR shifts were calculated and compared to the experimental results. The decomposition temperatures and the impact and friction sensitivities of these compounds have been determined as well.

Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Comprehensive Characterization

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.

scholarly journals Synthesis and Characterization of New Silver (I) N-Heterocyclic Ccarbene Ccomplex Dderived from Imidazol-2-ylidene salt

2018 ◽  
Vol 28 (2) ◽  
pp. 55
Author(s):  
Mohammedl Mujbe Hasson
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
13C Nmr ◽  
Room Temperature ◽  
13C Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Imidazolium Salt ◽  
In Situ Method

A new N, N'-imidazolium salt 1-(2,6-diisopropylphenyl)-3- (4,6-dimorpholino -1,3,5-traizine-2-yl)-1H-imidazol-3-ium chloride) as a precursor of N - heterocyclic carbene ligand was prepared via the reaction of 1 - (2, 6 - diisopropyl phenyl - 1H - imidazole) with 1, 3, 5 - triazine derivative bearing morpholine substituent (2, 6 -dimorpholine - 6- chloro-1, 3, 5-triaziazine). Linear coordi-nated Ag (І) NHC complex was synthesised via deprotonation of the imidazolium salt and reac-tion with Ag2O in darkness at room temperature by in situ method. The complex was synthesised for using as transfer agent to prepare another transition metals complexes by transmetallation method in the future. The imidazolium salt and their silver complex have been characterized by 1 H and 13C NMR spectroscopy as well as mass spectrometry.

Nine-Vertex Polyhedral Monoazaborane Chemistry: Synthesis and NMR Characterization of exo-6-Ligand-arachno-4-azanonaboranes(11), 6-L-4-NB8H11

1994 ◽  
Vol 59 (10) ◽  
pp. 2244-2252 ◽  
Author(s):  
Tomáš Jelínek ◽  
Bohumil Štíbr ◽  
John D. Kennedy
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Lewis Bases ◽  
H Nmr ◽  
Nmr Characterization ◽  
Complete Assignment

Reactions between arachno-4-NB8H13 and Lewis bases L in dichloromethane or without solvent generate the previously unreported series of arachno compounds exo-6-L-arachno-4-NB8H11, where L = pyridine (py), quinoline (quin), isoquinoline (i-quin), urotropine (uro), and MeCN. These are characterized by mass spectrometry together with 11B and 1H NMR spectroscopy. The NMR results permit complete assignment of all resonances and thence permit comparison with the structurally similar compounds exo-6-L-arachno-4-EB8H10 (for E = CH2 or S).

A combined 1H-NMR spectroscopy- and mass spectrometry-based metabolomic study of the PPAR-α null mutant mouse defines profound systemic changes in metabolism linked to the metabolic syndrome

2006 ◽  
Vol 27 (2) ◽  
pp. 178-186 ◽  
Author(s):  
Helen J. Atherton ◽  
Nigel J. Bailey ◽  
Wen Zhang ◽  
John Taylor ◽  
Hilary Major ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Metabolic Syndrome ◽  
Adipose Tissue ◽  
Nmr Spectroscopy ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
H Nmr ◽  
The Metabolic Syndrome ◽  
Chromatography Mass Spectrometry ◽  
Metabolic Role

The mobilization of triacylglycerides from storage in adipocytes to the liver is a vital response to the fasting state in mammalian metabolism. This is accompanied by a rapid translational activation of genes encoding mitochondrial, microsomal, and peroxisomal β-oxidation in the liver, in part under the regulation of peroxisome proliferator-activated receptor-α (PPAR-α). A failure to express PPAR-α results in profound metabolic perturbations in muscle tissue as well as the liver. These changes represent a number of deficits that accompany diabetes, dyslipidemia, and the metabolic syndrome. In this study, the metabolic role of PPAR-α has been investigated in heart, skeletal muscle, liver, and adipose tissue of PPAR-α null mice at 1 mo of age using metabolomics. To maximize the coverage of the metabolome in these tissues, 1H-NMR spectroscopy, magic angle spinning 1H-NMR spectroscopy, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry were used to examine metabolites in aqueous tissue extracts and intact tissue. The data were analyzed by the multivariate approaches of principal components analysis and partial least squares. Across all tissues, there was a profound decrease in glucose and a number of amino acids, including glutamine and alanine, and an increase in lactate, demonstrating that a failure to express PPAR-α results in perturbations in glycolysis, the citric acid cycle, and gluconeogenesis. Furthermore, despite PPAR-α being weakly expressed in adipose tissue, a profound metabolic perturbation was detected in this tissue.

Cucurbit[7]uril host-guest complexes with cationic bis(4,5-dihydro-1H-imidazol-2-yl) guests in aqueous solution

2006 ◽  
Vol 84 (6) ◽  
pp. 905-914 ◽  
Author(s):  
D Saroja N Hettiarachchi ◽  
Donal H Macartney
Keyword(s):  
Mass Spectrometry ◽  
Aqueous Solution ◽  
Nmr Spectroscopy ◽  
Stability Constants ◽  
Electrospray Mass Spectrometry ◽  
Hydrophobic Core ◽  
Guest Complex ◽  
H Nmr ◽  
Host Guest Complex ◽  
Proton Resonances

The host–guest interactions between cucurbit[7]uril and a series of novel cationic bis(4,5-dihydro-1H-imidazol-2-yl)arene and 1-(4,5-dihydro-1H-imidazol-2-yl)- and 1,3-bis(4,5-dihydro-1H-imidazol-2-yl)-adamantane guests have been investigated in aqueous solution using UV–vis and NMR spectroscopy, and electrospray mass spectrometry. With the exception of the 1,3-bis(4,5-dihydro-1H-imidazol-2-yl)adamantane (which binds externally to the CB[7]), these guests form very stable inclusion complexes with slow exchange on the 1H NMR timescale. The direction and magnitude of the complexation-induced shifts (CIS) in the proton resonances of the guests are indicative of the residence of the hydrophobic core of the guest within the CB[7] cavity and the charged 4,5-dihydro-1H-imidazol-2-yl units outside the cavity adjacent to the carbonyl-lined portals of the host. The CIS values and the inclusion stability constants have been correlated with the nature of the guest core and with the distance between the charges on the terminal 4,5-dihydro-1H-imidazol-2-yl rings.Key words: cucurbit[7]uril, host–guest complex, dihydroimidazolyl, inclusion stability constants.

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