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 Silver(I) and Gold(I) Complexes Bearing a Pyrido-annelated N-Heterocyclic Carbene: A Rare Example of a Cocrystal Containing Two Different Gold(I) Complexes

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1188-1198 ◽  
Author(s):  
Margit Kriechbaum ◽  
Daniela Otte ◽  
Manuela List ◽  
Uwe Monkowius
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Aromatic Compound ◽  
Elemental Analysis ◽  
Room Temperature ◽  
Electronic Spectroscopy ◽  
Crystalline Material ◽  
Synthesis And Characterization ◽  
Aurophilic Interactions

Abstract The cyclohexyl-substituted imidazo[1,5-a]pyridin-2-ium hexafluorophosphate, 2a, has been prepared as precursor for the respective pyrido-annelated N-heterocyclic carbene. [(NHC)2Ag]PF6, 3, has been synthesized by the reaction of 2a with AgCl=KOH in dichloromethane (DCM). Unexpectedly, the reaction of 3 with (tht)AuBr yielded both (NHC)AuBr and [(NHC)Au(tht)]PF6 which formed a 1 : 1 cocrystal (4a,b). The complexes are aggregated to infinite chains, which are governed by both π-π stacking and weak aurophilic interactions. Subsequent oxidation of the co-crystalline material with CsBr3 gave (NHC)AuBr3, 5. All compounds were characterized by NMR spectroscopy, mass spectrometry and elemental analysis. Additionally, compounds 2a and 5 were investigated by electronic spectroscopy: 2a behaves like a typical aromatic compound exhibiting absorption and fluorescence bands attributable to π-π* transitions. The Au(III) complex 5 exhibits ligand-centered fluorescence at room temperature and both ligand-centered fluorescence and a weak phosphorescence at 77 K.

scholarly journals Synthesis and characterization of new Oxazine , Thiazine and Pyrazol derived from chalcones

2014 ◽  
Vol 11 (2) ◽  
pp. 477-485 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrazine Hydrate ◽  
Elemental Analysis ◽  
Potassium Hydroxide ◽  
1H Nmr Spectroscopy ◽  
Room Temperature ◽  
Potassium Hydroxide Solution ◽  
Synthesis And Characterization ◽  
Heterocyclic Derivatives

In this study, chalcones were synthesis by condensing 2-acetylpyridine with aromatic aldehyde derivatives in dilute ethanolic potassium hydroxide solution at room temperature according to Claisen-Schmidt condensation. After that, new heterocyclic derivatives such as Oxazine, Thiazine and Pyrazol were synthesis by reaction between chalcones with urea, thiourea and hydrazine hydrate respectively scheme 1. All these compounds wrer characterization by FTIR, 1H-NMR spectroscopy and elemental analysis.

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.

Synthesis and Characterization of the nido-Platinaborane 7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me

2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reaction of closo-B10H102− with PtCl2(PPh3)2 in the presence of MeCOSH afforded the title platinaborane nido-7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me (1), which has been characterized by IR and NMR spectroscopy, MS, elemental analysis, and single-crystal X-ray diffraction. In contrast to the known products having exo-polyhedral Pt-S-C-O-B ring(s) from the same reaction with Ph- COSH, compound 1 has a B-acetoxy group on the open PtB4 face of the nido-PtB10 cluster. The structure of 1 features both intramolecular/intermolecular C-H· · ·O hydrogen bonds and intramolecular C-H· · ·H-B dihydrogen bonds, which link the molecules into a 1-D chain structure.

scholarly journals Synthesis and Characterization of New Optically Active Poly (ethyl L-lysinamide)s and Poly (ethyl L-lysinimide)s

2010 ◽  
Vol 2010 ◽  
pp. 1-6 ◽  
Author(s):  
Saeed Zahmatkesh ◽  
Mohammad Reza Vakili
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Specific Rotation ◽  
Viscosity Measurement ◽  
Optically Active ◽  
Inherent Viscosity ◽  
Synthesis And Characterization

Ethyl L-lysine dihydrochloride was reacted with three different dianhydrides to yield the poly (ethyl L-lysinimide)s ( NMR spectroscopy, elemental analysis, WAX diffraction, TGA, inherent viscosity measurement, and specific rotation.

Chemistry of the 1,3,5-Triaza-2-phosphorin-4,6-diones, Part XII*. Synthesis and Characterization of 2-PhenyI-2-(p-tolylthio)-1,3,5- trimethyI-1,3,5-triaza-4,6-dione-2-phosphorinonium Salts

1996 ◽  
Vol 51 (10) ◽  
pp. 1494-1500 ◽  
Author(s):  
Vasily A . Pinchuk ◽  
Ion Neda ◽  
Christian Müller ◽  
Holger Thönnessen ◽  
Peter G. Jones ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
New Products ◽  
Synthesis And Characterization ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Weak Hydrogen Bonds ◽  
C Nmr

The reaction of 1,5-bis(trimethylsilyl)-1,3.5-trimethylbiuret (1) with p-tolylsulfenyl chloride (2) furnished l-(p-tolylthio)-5-trimethylsilyl-1,3,5-trimethylbiuret (3). In the reaction of 3 with phenyldichlorophosphine, 2-phenyl-2-(p-tolylthio)-1,3,5-trimethyl-1,3,5-triaza-4,6-dione- 2-phosphorinonium chloride (4) was formed. The same product was obtained from the reaction of 2-phenyl-1,3,5-trimethyl-1,3,5-triaza-2λ3- phosphorin-4,6-dione (6) with p-tolylsulfenyl chloride (2). Compound 4 was isolated and characterized in the form of the hexachloroantimonate (4a). The spirophosphorane 2-phenyl-1,3,5-trimethyl-1,3,5-triaza-7,10-dioxa-8,9- perchlorobenzo-2λ5-phosphaspiro-[4.5]decan-4,6-dione (7) was prepared by the reaction of 4 with tetrachloroorthobenzoquinone. The new products were characterized by 1H - and 13C NMR spectroscopy, elemental analysis, 31P NMR spectroscopy in the case of 4a. 6 and 7, and mass spectrometry (4a). Single-crystal X-ray structural analyses of compounds 4a and 7 were conducted. The phosphorus atom of 4a has the expected tetrahedral geometry, with a rather short P-S bond of 204.9(2) pm. In 7 the geometry at phosphorus is almost ideal trigonal bipyramidal. Weak hydrogen bonds are formed from a C (:O) group to deuterochloroform of solvation.

scholarly journals Synthesis and characterization of palladium(II) complexes with glycine coumarin derivatives

2016 ◽  
Vol 81 (12) ◽  
pp. 1383-1392
Author(s):  
Danijela Stojkovic ◽  
Alessia Bacchi ◽  
Davide Capucci ◽  
Milica Milenkovic ◽  
Bozidar Cobeljic ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Water Solution ◽  
13C Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Coumarin Derivatives ◽  
1H And 13C Nmr ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

A Pd(II) complex with methyl 2-((1-(2,4-dioxochroman-3-ylidene)ethyl)amino)acetate was synthesized. The structures of both the ligand and Pd(II) complex were determined by elemental analysis, IR and NMR spectroscopy. Recrystallization of Pd(II) complex from DMF/water solution resulted in its hydrolysis and formation of dimethylamine-(2-((1-(2,4-dioxochroman-3-ylidene)ethyl)amino)acetato)palladium(II) complex, the structure of which was determined by elemental analysis, IR, 1H and 13C NMR spectroscopy, as well as X-ray analysis.

scholarly journals Synthesis and characterization of tris[butyl-(1-methyl-3phenyl-propyl)-dithiocarbamato]cobalt(III) seskvitoluen

2002 ◽  
Vol 67 (2) ◽  
pp. 123-126 ◽  
Author(s):  
Goran Kaludjerovic ◽  
Vesna Djinovic ◽  
Srecko Trifunovic ◽  
Ismet Hodzic ◽  
Tibor Sabo
Keyword(s):  
Nmr Spectroscopy ◽  
Electronic Absorption ◽  
Elemental Analysis ◽  
13C Nmr ◽  
Sodium Salt ◽  
13C Nmr Spectroscopy ◽  
Bidentate Ligand ◽  
Synthesis And Characterization ◽  
1H And 13C Nmr

Anew bidentate ligand butyl-(1-methyl-3-phenyl-propyl)-dithiocarbamate (bm?pdtc) was prepared, as the sodium salt. In the reaction of hexaaminecobalt(III) chloride with Nabm?pdtc, the corresponding tris[butyl-(1-methyl-3-phenyl-propyl)-dithiocarbamato]cobalt(III) [Co(bm?pdtc)3]?complex was prepared. The complex was characterized by elemental analysis, infrared, electronic absorption, 1H and 13C-NMR spectroscopy.

Synthesis and Structural Characterization of Metal Complexes of 2-Formylpyrrole 4N-Methylthiosemicarbazone (4ML1) and 2-Acetyl- pyrrole 4N-Methylthiosemicarbazone (4ML2). The X-Ray Crystal Structures of [Ni(4ML1-H)2], [Pd(4ML1-H)2] and [Cd(4ML2)2I2]

2001 ◽  
Vol 56 (3) ◽  
pp. 219-228 ◽  
Author(s):  
Ruben Alonso ◽  
Elena Bermejo ◽  
Rosa Carballo ◽  
Alfonso astiñeiras ◽  
Teresa Pérez
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Structural Characterization ◽  
X Ray ◽  
Group 12 ◽  
New Compounds ◽  
Group 10 Metals ◽  
C Nmr

Abstract Reaction of 4N-methyl-2-[1-(pyrrol-2-yl)methylidene]hydrazinecarbothioamide (4ML1 and 4N-methyl-2-[1-(pyrrol-2-yl)-ethylidene]hydrazine carbothioamide (4ML1) with zinc(II), cadmium(II) and mercury(II) halides afforded complexes with formulas [M(L)X2] [(L; M; X) =(4ML1; Cd; Cl) (4), (4ML1; Hg; Cl, Br, I) (7 - 9), (4ML2; Cd; Cl) (17), (4ML2; Hg; Cl, Br, I) (20 - 22)] or [M(L)2X2] [(L; M; X) = (4ML1; Zn; Cl, Br, I) (1 - 3), (4ML1; Cd; Br, I) (5, 6), (4ML2; Zn; Cl, Br, I) (14 - 16), (4ML2; Cd; Br, I) (18, 19)]. Reaction of 4ML1 with salts of copper(II), nickel(II), palladium(II) and platinum(II) afforded complexes of formula [M(4ML1-H)2] (10 -13). Crystals of 11, 12 and 19 were studied by X-ray diffractometry, and all new compounds were characterized by elemental analysis, mass spectrometry, and IR, electronic and 1H and 13C NMR spectroscopy and, when pertinent and allowed by the solubility of the compound, 113Cd or 199Hg NMR spectroscopy. In the complexes of Group 12 metals, both ligands are neutral and S-monodentate. In the complexes of copper or Group 10 metals, 4ML1 is monodeprotonated and S,N-bidentate.

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