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).

scholarly journals Copolymer chain formation of 2-oxazolines by in situ1H-NMR spectroscopy: dependence of sequential composition on substituent structure and monomer ratios

RSC Advances ◽  
2021 ◽  
Vol 11 (18) ◽  
pp. 10468-10478
Author(s):  
Sabina Abbrent ◽  
Andrii Mahun ◽  
Miroslava Dušková Smrčková ◽  
Libor Kobera ◽  
Rafał Konefał ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Polymer Chains ◽  
Chain Formation ◽  
Molar Ratios ◽  
H Nmr ◽  
Copolymer Chain ◽  
Nmr Characterization ◽  
Insight Into

In situ1H NMR characterization of copolymerization reactions of various 2-oxazoline monomers at different molar ratios offers detailed insight into the build-up and composition of the polymer chains.

Synthesis, Separation and Characterization of Naphthobenzo-condensed Porphyrazinato Nickel(II) Complexes

1997 ◽  
Vol 01 (02) ◽  
pp. 169-179 ◽  
Author(s):  
RAINER POLLEY ◽  
TORSTEN GOLO LINßEN ◽  
PATRICK STIHLER ◽  
MICHAEL HANACK
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Column Chromatography ◽  
Potential Importance ◽  
Macrocyclic Compounds ◽  
H Nmr ◽  
Advanced Technologies ◽  
Benzene Rings

Phthalocyanines and 2,3-naphthalocyanines are macrocyclic compounds which possess a variety of properties of potential importance in advanced technologies. The article discusses the influence of successive condensation of additional benzene rings to the phthalocyanine system. For this purpose three hexyloxy- and heptyl-substituted 2,3-dicyanonaphthalenes 3,7,11 and the respective 2,3-naphthalocyaninato nickel(II) complexes were prepared. In three statistical condensations of tetraphenylphthalodinitrile ( TPPN ) (12) and 2,3-dicyanonaphthalenes, 3,7,11, twelve unsymmetrical naphthobenzo-condensed porphyrazinato nickel(II) complexes 13b-15e were synthesized and separated by common column chromatography. All complexes were characterized by mass spectrometry, IR, UV and 1 H NMR spectroscopy.

A twist on Hellwinkel’s salt, [P(2,2′-biphenyl)2]+[P(2,2′-biphenyl)3]–

2018 ◽  
Vol 96 (6) ◽  
pp. 526-533 ◽  
Author(s):  
Khatera Hazin ◽  
Derek P. Gates
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Spiro Compound ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Isolation And Characterization

Treating PCl5 with C12H8Li2, generated from either C12H10, C12H8Br2, or C12H8I2, affords three products in different ratios depending on the source of the lithiated biphenyl. Hellwinkel’s salt [P(C12H8)2][P(C12H8)3] ([1][2]) and another product [P(C12H8)(C24H16)][P(C12H8)3] ([1′][2]) were obtained by reacting PCl5 with 2,2′-dilithiobiphenyl [Route A: 2.5 equiv.; obtained from biphenyl, n-BuLi, and TMEDA; Route B: 3.0 equiv.; obtained from 2,2′-diiodobiphenyl and n-BuLi; Route C: 4.0 equiv.; obtained from 2,2′-dibromobiphenyl and n-BuLi]. The synthesis, isolation, and characterization of the chiral spiro-compound [1′][2] and the characterization of the pentavalent phosphorane [P(C12H8)2(C12H9)] (3) are reported. The complex [1′][2] was characterized by 31P{1H} NMR spectroscopy, X-ray crystallography, and mass spectrometry. The pentavalent compound (3) was characterized by 31P{1H} NMR spectroscopy and X-ray crystallography.

scholarly journals Characterization of the synthetic cannabinoid MDMB-CHMCZCA

2016 ◽  
Vol 12 ◽  
pp. 2808-2815 ◽  
Author(s):  
Carina Weber ◽  
Stefan Pusch ◽  
Dieter Schollmeyer ◽  
Sascha Münster-Müller ◽  
Michael Pütz ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Hplc Method ◽  
Enantiomeric Purity ◽  
Synthetic Cannabinoid ◽  
Spectroscopic Techniques ◽  
Chiral Hplc ◽  
Tandem Mass ◽  
Synthetic Sample

The synthetic cannabinoid MDMB-CHMCZCA was characterized by various spectroscopic techniques including NMR spectroscopy and tandem mass spectrometry. The synthetic sample was found to be of S-configuration by VCD spectroscopy and comparison of the data with DFT calculations, while ECD spectroscopy was found to be inconclusive in this case. The enantiomeric purity of samples from test purchases and police seizures was assessed by a self-developed chiral HPLC method.

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.

Synthesis and characterization of a new (phthalocyani-nato)bis(carboxylate) silicon(IV) compound with increased solubility

2002 ◽  
Vol 06 (03) ◽  
pp. 198-202 ◽  
Author(s):  
José L. Sosa-Sánchez ◽  
Alberto Galindo ◽  
Dino Gnecco ◽  
Sylvain Bernès ◽  
George R. Fern ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Structure Determination ◽  
Spectroscopic Characterization ◽  
X Ray Diffraction ◽  
H Nmr ◽  
Axial Ligands ◽  
Nmr Characterization ◽  
Soluble Silicon ◽  
Soluble Material

The synthesis and spectroscopic characterization of a new soluble silicon(IV) phthalocyanine complex is presented. The compound shows an increased solubility compared to its SiPcCl 2 precursor and this allowed solution 1 H NMR characterization. The assignment of the 1 H NMR signals for the axial ligands is greatly facilitated due to the anisotropic high ring current effects from the macrocycle. In addition, good quality crystals were grown from this more soluble material for molecular structure determination by single-crystal X-ray diffraction analysis. The molecular structure determination shows that the complex crystallizes in a non-centrosymmetric space group due to the inherent chirality of the naproxene ligands. Bond lengths and angles fit well to other analogous compounds previously reported.

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.

Nine- and Eight-Vertex Polyhedral Dicarbaborane Chemistry: New arachno and hypho Dicarbaboranes from arachno-4,5-C2B7H13: Isolation and Characterization of the [arachno-4,5-C2B7H12]- and [hypho-7,8-C2B6H13]- Anions, and of the Neutral Ligand Derivatives exo-6-(MeNC)-arachno-4,5-C2B7H11 and exo-5-L-hypho-4,9-C2B7H13 (L = NMe3 and NEt3)

1994 ◽  
Vol 59 (7) ◽  
pp. 1584-1595 ◽  
Author(s):  
Tomáš Jelínek ◽  
Josef Holub ◽  
Bohumil Štíbr ◽  
Xavier L. R. Fontaine ◽  
John D. Kennedy
Keyword(s):  
Nmr Spectroscopy ◽  
Selective Removal ◽  
High Yield ◽  
Two Dimensional ◽  
Neutral Ligand ◽  
Tertiary Amines ◽  
Proton Sponge ◽  
H Nmr ◽  
Isolation And Characterization

Deprotonation of neutral arachno-4,5-C2B7H13 (1) either with 1, 8-(NMe2)2C10H6 (proton sponge, PS) or with a mixture of aqueous K2CO3 and [NMe4]Cl leads to the isolation in high yield of the [arachno-4,5-C2B7H12]- anion (2). Isostructural with this anion is the ligand derivative exo-6-(MeNC)-arachno-4,5-C2B7H11 (3), which is prepared in 20% yield from the reaction between arachno-4,5-C2B7H13 and MeNC in dichloromethane. Under comparable conditions compound 1 with tertiary amines gives the first representatives of the nine-vertex hypho family of dicarbaboranes, the ligand derivatives exo-5-(NR3)-hypho-4,9-C2B7H13 (4a and 4b, where R = Me and Et, respectively) in moderate yields (20 - 55%), whereas the reaction between 1 and aqueous NaCN results in the selective removal of one boron vertex to yield the eight-vertex [hypho-7,8-C2B6H13]- anion (5) in 61% yield. All compounds isolated were characterized by 11B and 1H NMR spectroscopy, with two-dimensional and selective decoupling techniques giving unambiguous assignments.

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