Synthesis and characterization of a series of 4-methyl-1-[2-aryl-1-diazenyl]-1,4-diazepanes and 1,4-di-[2-aryl-1-diazenyl]-1,4-diazepanes

2004 ◽  
Vol 82 (12) ◽  
pp. 1725-1735 ◽  
Author(s):  
Shasta Lee Moser ◽  
Keith Vaughan
Keyword(s):  
Nmr Assignments ◽  
Diazonium Salt ◽  
Variable Temperature ◽  
2D Nmr ◽  
Diazonium Salts ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds ◽  
C Nmr

1-Methylhomopiperazine was coupled with a series of diazonium salts to afford the 4-methyl-1-[2-aryl-1-diazenyl]-1,4-diazepanes (6), a new series of triazenes. These compounds are, in the main, stable crystalline solids (some of the series are stable oils), and they have been characterized by 1H and 13C NMR spectroscopy, IR spectroscopy, and mass spectrometry. NMR assignments were determined by 2D NMR and variable-temperature NMR experiments and by comparison with model compounds. A second series of new compounds, namely, 1,4-di-[2-aryl-1-diazenyl]-1,4-diazepanes (5), were prepared by coupling unsubstituted homopiperazine (1,4-diazepane) with 2 molar equivalents of the diazonium salt and were similarly characterized. The crystal and molecular structure of the parent member of this bis-triazene series (5, X = H) has been determined by single-crystal X-ray diffraction analysis.Key words: triazene, bis-triazene, diazenyl, bis-diazenyl, diazonium salt, NMR, diazepane.

N-alkyl-2-(1,2-diferrocenylvinyl)-4,5-dihydrooxazolinium salts, multi-component synthesis and breaking of their heterocyclic systems

2016 ◽  
Vol 88 (12) ◽  
pp. 1129-1142 ◽  
Author(s):  
Jessica J. Sánchez García ◽  
Marcos Flores-Alamo ◽  
Mark E. Martínez Klimov ◽  
Elena I. Klimova
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Alkyl Iodides ◽  
New Compounds ◽  
C Nmr

AbstractA new multicomponent method for the synthesis of N-alkyl-2-(Z-1,2-diferrocenylvinyl)-4,5-dihydrooxazolinium salts 3a–f, 5-(N-alkyl-2′,3′-diferrocenyl-acryloylamido)-3-aza-3-alkylpentanols 4a–d, (E)-N-alkyl-N-(2-morpholinoethyl)-2,3-diferrocenylacrylamides 9a,b,e,f and (E)-N-alkyl-N-(2-piperidinoethyl)-2,3-diferrocenylacrylamides 10a,c from reactions of 2,3-diferrocenylcyclopropenone 1 with bis-1,4-N,O-nucleophiles in the presence of triethyloxonium tetrafluoroborate, alkyl iodides, morpholine, piperidine and Et3N is described. The characterization of the new compounds was done by IR, 1H- and 13C-NMR spectroscopy, mass-spectrometry, elemental analysis and X-ray diffraction studies.

Star mesogens — Synthesis and structural characterization using 1D and 2D solution NMR techniques and mesophase characterization

2013 ◽  
Vol 91 (3) ◽  
pp. 196-205 ◽  
Author(s):  
A. Shanavas ◽  
T. Narasimhaswamy ◽  
B.V.N. Phani Kumar ◽  
A. Sultan Nasar
Keyword(s):  
Chain Length ◽  
Liquid Crystalline ◽  
Variable Temperature ◽  
2D Nmr ◽  
Smectic Layer ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Xrd Techniques ◽  
Terminal Chain

Novel star mesogens based on trimesic acid and symmetrical side arm cores with terminal alkoxy groups were synthesized via a divergent approach. The central core and side arms were connected through alkyl spacers. All the synthesized mesogens and their intermediates were characterized thoroughly using Fourier transform infrared (FT-IR), 1H nuclear magnetic resonance (NMR), 13C NMR, and mass spectrometers. One representative mesogen was subjected to the two-dimensional (2D) NMR experiments to ascertain the structure of the mesogens. The mesophase characterization was carried out using hot-stage optical polarizing microscopy (HOPM), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques. Many of the molecules with an ethyloxy spacer were found to be nonmesogenic, whereas all the molecules with a butyloxy spacer showed liquid crystalline phases. The increase of terminal chain length decreased the transition temperatures. The nematic phase was observed for the mesogens with short terminal chain length, whereas smectic polymorphism was observed on increasing the terminal chain length. The results of a variable temperature powder X-ray diffraction of the representative sample support the smectic layer ordering.

Article

1999 ◽  
Vol 77 (5-6) ◽  
pp. 1057-1065
Author(s):  
John T Edward ◽  
Francis L Chubb ◽  
Denis FR Gilson ◽  
Rosemary C Hynes ◽  
Françoise Sauriol ◽  
...  
Keyword(s):  
Nmr Spectra ◽  
Acidic Solution ◽  
Variable Temperature ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
Cage Compounds ◽  
Amine Nitrogen ◽  
X Ray ◽  
Bridgehead Nitrogen ◽  
C Nmr

Three new cage peroxides, 1,6-diaza-3,4,8,9-tetraoxabicyclo[4.4.2]dodecane (3a),1,6-diaza-3,4,8,9-tetraoxa-11-methylbicyclo[4.4.2]dodecane (3b), and 1,6-diaza-3,4,8,9-tetraoxatricyclo[4.4.2.411,12]hexadecane (4), have been prepared by reaction of 1,2-diaminoethane, 1,2-diaminopropane, and trans-1,2-diaminocyclohexane, respectively, with formaldehyde and hydrogen peroxide in aqueous acidic solution. Their structures have been established by X-ray diffraction, and show the bridgehead nitrogen atoms to be predominantly sp2 hybridized. The structures accord with 1H and 13C NMR spectra. Variable temperature NMR studies show that the diperoxide 3a begins to undergo rapid inversion (on the NMR time scale) at about 303 K; up to 370 K the diperoxides 3b and 4 show no conformational change.Key words: cage compounds, formaldehyde, peroxides, amine nitrogen, hybridization.

The Effects of Substrate-Induced Strains on the Charge-Ordering Transition in Nd0.5Sr0.5MnO3 Thin Films

1999 ◽  
Vol 602 ◽  
Author(s):  
W. Prellier ◽  
Amlan Biswas ◽  
M. Rajeswari ◽  
T. Venkatesan ◽  
R.L. Greene
Keyword(s):  
Thin Films ◽  
Variable Temperature ◽  
Charge Ordering ◽  
Laser Deposition ◽  
X Ray Diffraction ◽  
Metallic Behavior ◽  
X Ray ◽  
Post Annealing ◽  
Ordering Transition

AbstractWe report the growth and characterization of Nd0.5Sr0.5MnO3 thin films deposited by the Pulsed Laser Deposition (PLD) technique on [100]-oriented LaAlO3 substrates. X-ray diffraction (XRD) studies show that the films are [101]-oriented, with a strained and quasi-relaxed component, the latter increasing with film thickness. A post-annealing under oxygen leads to a quasi-relaxed film with a metallic behavior. We also observe that transport properties are strongly dependent on the thickness of the films. Variable temperature XRD down to 100 K suggests that this is caused by substrate-induced strain on the films.

Structural characterization of p-benzosemiquinone radical in a solid state: the radical stabilization by a low-barrier hydrogen bond

2006 ◽  
Vol 62 (6) ◽  
pp. 1051-1060 ◽  
Author(s):  
Krešimir Molčanov ◽  
Biserka Kojić-Prodić ◽  
Mario Roboz
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Variable Temperature ◽  
Organic Radical ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Packings ◽  
Dynamical Disorder ◽  
Benzenoid Ring

Semiquinone (p-benzosemiquinone), a transient organic radical, was detected in the solid state by EPR spectroscopy revealing four symmetrically equivalent protons. A variable-temperature X-ray diffraction analysis (293 and 90 K) and EPR data support a dynamical disorder of the proton. A low-barrier O—H···O hydrogen bond stabilizes the radical. The C—O bond length is 1.297 (4) Å, corresponding to a bond order of ca 1.5. The geometry of the radical implies an electron delocalization throughout the benzenoid ring. Two polymorphs of semiquinone, monoclinic and triclinic, were observed and their structures determined. Their crystal packings were compared with those of quinhydrone polymorphs.

scholarly journals Synthesis and characterization of allyl- and vinyl-substituted 1,2-bis(tetrazolo)ethanes as polymeric precursors

2016 ◽  
Vol 71 (12) ◽  
pp. 1199-1209
Author(s):  
Vera A. Hartdegen ◽  
Maximilian S. Hofmayer ◽  
Konstantin Karaghiosoff ◽  
Thomas M. Klapötke
Keyword(s):  
Allyl Bromide ◽  
2D Nmr ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
2D Nmr Spectroscopy ◽  
X Ray ◽  
Physical Stimuli ◽  
Thermal Stability Of

AbstractOn the basis of 1,2-bis(5-tetrazolo)ethane (BTE) the corresponding twofold vinyl and allyl N-substituted derivatives were synthesized using 1,2-dibromoethane and allyl bromide, respectively. The compounds were obtained as two different constitutional isomers. Both species were analyzed using NMR and IR spectroscopy, elemental analysis, as well as mass spectrometry. In the case of the diallyl bistetrazoles, the two isomers were characterized using 2D NMR spectroscopy. The synthesis of the divinyl compounds gave crystals of the 2,2′-N-substituted isomer, which were analyzed by single-crystal X-ray diffraction. The thermal stability of the compounds was determined using differential scanning calorimetry (DSC) and gave decomposition temperatures around 190°C and 230°C. For the investigation of the inherent energetic potential, sensitivities toward physical stimuli and detonation parameters were determined. The compounds turned out to be insensitive toward friction and impact and possess moderate energetic properties.

Synthesis and structural characterization of substituted phenols with a m-terphenyl backbone 2,4,6-R3C6H2OH (R=2,4,6-Me3C6H2, Me5C6)

2015 ◽  
Vol 70 (1) ◽  
pp. 77-81 ◽  
Author(s):  
Atena B. Şolea ◽  
Marian Olaru ◽  
Cristian Silvestru ◽  
Ciprian I. Raţ
Keyword(s):  
Grignard Reagent ◽  
Cross Coupling ◽  
Molecular Structures ◽  
Coupling Reactions ◽  
X Ray Diffraction ◽  
Substituted Phenols ◽  
X Ray ◽  
Cross Coupling Reactions ◽  
C Nmr

AbstractSubstituted phenols with a m-terphenyl backbone 2,4,6-R3C6H2OH [R=2,4,6-Me3C6H2 (1), Me5C6 (2)] were synthesized using Kumada cross-coupling reactions between 2,4,6-I3C6H2OH and the corresponding Grignard reagent. Both compounds were structurally characterized in solution by 1H and 13C NMR spectroscopy and HRMS. The molecular structures of 1 and 2 were determined by single-crystal X-ray diffraction.

Synthese und röntgenographische Charakterisierung von zwei neuen Verbindungen des Ludwigit-Strukturtyps: Co5Sn(BO3)2O4 und Co5Mn(BO3 )2O4/Synthesis and X -Ray Characterization of Two New Compounds with Ludwigite-Structure: Co5Sn(BO3)2O4 and Co5Mn(BO3)2O4

1996 ◽  
Vol 51 (3) ◽  
pp. 305-308 ◽  
Author(s):  
Anne Utzolino ◽  
Karsten Bluhm
Keyword(s):  
Orthorhombic Symmetry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxygen Coordination ◽  
New Compounds ◽  
Octahedral Oxygen ◽  
Group D ◽  
Symmetry Space ◽  
Symmetry Space Group

Abstract The compounds Co5Sn(BO3)2O4 (I) and Co5Mn(BO3)2O4 (II) were prepared by using a B2O3 flux technique. Single crystals were investigated by X-ray diffraction and showed orthorhombic symmetry, space group D2h9-Pbam (No. 55), I a = 944.4; b = 1233.8; c = 310.5 pm; Z = 2 and II a = 925.07; b = 1241.67; c = 305.24 pm; Z = 2. Both compounds are isotypic to the mineral Ludwigite. All metal point positions show an octahedral oxygen coordination. Co2+ and M4+ (M = Sn or Mn) occupy one point position statistically. Both structures contain isolated, trigonal planar BO3 units and oxygen atoms that are not coordinated to boron.

Synthesis and Pharmacological Evaluation of a Novel Series of Cyclopentenone Derivatives

2017 ◽  
Vol 41 (1) ◽  
pp. 50-56 ◽  
Author(s):  
Fatma A. El-Samahy ◽  
Marwa El-Hussieny ◽  
Naglaa F. El-Sayed ◽  
Elsayed M. Shalaby ◽  
Fayez H. Osman
Keyword(s):  
Mass Spectra ◽  
Secondary Amines ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Chemical Structures ◽  
Pharmacological Evaluation ◽  
New Compounds ◽  
C Nmr ◽  
Boiling Toluene

A novel series of cyclopent-2-enone derivatives have been synthesised by the reaction of 4-hydroxy-3,4-diphenylcyclopent-2-enone, cyclic secondary amines, phosphorus reagents, hexamethylphosphoramide and Lawesson's reagent in boiling toluene/THF. The chemical structures of new compounds were identified by 1H NMR, 13C NMR, 31P NMR and mass spectra. Furthermore, the structure of one of the synthesised compounds has been confirmed using single crystal X-ray diffraction. The pharmacological evaluation results of antilung and anticolon carcinoma cell line properties for the products are discussed.

Sign in / Sign up

Export Citation Format

Share Document