Synthesis and Characterization of Three Novel Nitrogen-containing Macrolides

2011 ◽  
Vol 66 (9) ◽  
pp. 930-934
Author(s):  
Xin Leng ◽  
Bingqin Yang ◽  
Yuanyuan Liu ◽  
Yi Xie ◽  
Jie Tong
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
1H Nmr Spectroscopy ◽  
Mass Spectra ◽  
Synthesis And Characterization ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
X Ray

Three novel nitrogen-containing macrolides have been synthesized by esterification. All of them have been characterized by infrared (IR), elemental analysis, mass spectra (MS), and 1H NMR spectroscopy, and their crystal structures were determined by single-crystal X-ray diffraction. The preparation methods and the intermolecular associations based on C-H・・・O hydrogen bonds and π- π stacking interactions are discussed.

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.

Microwave-assisted solvent-free synthesis and spectral and structural characterization of cyclotriphosphazene hexakis(o-tolylamide)

2018 ◽  
Vol 73 (12) ◽  
pp. 999-1003 ◽  
Author(s):  
Mohammad Hakimi ◽  
Homeyra Rezaei ◽  
Keyvan Moeini ◽  
Heidar Raissi ◽  
Vaclav Eigner ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Microwave Irradiation ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
Microwave Assisted ◽  
Ft Ir ◽  
Solvent Free Synthesis

AbstractA new cyclotriphosphazene, 2,2,4,4,6,6-hexakis (o-tolylamono)-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinine (MPAP), was prepared using microwave irradiation and identified by elemental analysis, FT-IR, Raman, 31P NMR spectroscopy, and single-crystal X-ray diffraction. In the crystal, in addition to hydrogen bonds, the network is further stabilized by inter- and intramolecular π–π stacking interactions between aromatic rings.

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.

Synthesis and characterization of dicarboranylmethylammonium polyoxometallates

2010 ◽  
Vol 75 (11) ◽  
pp. 1075-1096 ◽  
Author(s):  
Ramón Macías ◽  
John D. Kennedy ◽  
Jonathan Bould ◽  
Mark Thornton-Pett
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridinium Cation ◽  
Network Of Hydrogen Bonds ◽  
Work Up ◽  
Acetone Hexane

The reaction of [C2B10H11CH2NH3]Cl (3) with [NH4]6[Mo7O24][H2O]4 in water instantly afforded a white precipitate: crystallization from acetone–hexane thence gave the hybrid dicarborane octamolybdate salt, [C2B10H11CH2NH3]2[C2B10H11CH2NH=CMe2]2[Mo8O26][Me2CO]4.5 (5), whereas crystallization from acetonitrile–ether gave three further salts: [C2B10H11CH2NH3]2[C2B10H11CH2NH2CHMe2]2[Mo8O26][MeCN]2 (6), [C2B10H11CH2NH3]4[Mo8O26][MeCN]2[Et2O]2 (7) and [C2B10H11CH2NH3]2[C2B10H11CH2NH2Et]2[Mo8O26][MeCN]2 (8). Similarly, treatment of an acidified solution of Na2WO4 with [C2B10H11CH2NH3]Cl (3) in water also yielded a white precipitate: crystallization from acetone–hexane afforded the salt [C2B10H11CH2NH=CHMe2]4[W10O32][H2O]2[Me2CO]4 (10), whereas crystallization from acetonitrile–ether gave the double salt [C2B10H11CH2NH3]2[C5H5NH]2[W10O32][MeCN]2-[Et2O] (11). All these ‘globule–globule’ salts 5, 6, 8, 10 and 11 have been characterized by single-crystal X-ray diffraction analyses. Crystal structures reveal the presence of various small solvate molecules, together with an extensive network of hydrogen bonds between ammonium groups and oxygen atoms of the isopolyoxometallates. The isopropyl substituent in one of the carborane cations of the salts 6 and the ethyl substituent in one of the carborane cations of salts 8 may result from occluded isopropanol and ethanol in the starting salt 3 with alkylations of the primary ammonium group being assisted by isopolymolybdate anions. The presence of the pyridinium cation in 11 is believed to arise from contamination during work-up the reaction mixture.

The Synthesis and Characterization of NiCo2O4 Nanoparticles

2012 ◽  
Vol 512-515 ◽  
pp. 2467-2470 ◽  
Author(s):  
Hong Xiao Zhao ◽  
Bao Ming He ◽  
Jing Li ◽  
Hui Min Jia ◽  
Li Wei Mi
Keyword(s):  
Thermal Decomposition ◽  
Hydrothermal Method ◽  
Physical Adsorption ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
Oxalate Precursor ◽  
X Ray ◽  
Scanning Electron

In this paper, NiCo2O4 nanoparticles were synthesized by three different methods. The applied preparation methods in this research are thermal decomposition of a mixed oxalate precursor, combustion synthesis and hydrothermal method. The crystalline phase, morphology and specific surface area (BET) of the resultant samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and nitrogen physical adsorption, respectively. The research found that the hydrothermal method is a promising method to prepare NiCo2O4 nanoparticles.

scholarly journals Palladium(II) complexes with R2edda derived ligands, Part III: Diisobutyl (s,s)-2,2'-(1,2-ethanediyldiimino)di(4-methylpentanoate) and its palladium(II) complex: Synthesis and characterization

2009 ◽  
Vol 74 (11) ◽  
pp. 1249-1258 ◽  
Author(s):  
Bojana Zmejkovski ◽  
Goran Kaludjerovic ◽  
Santiago Gómez-Ruiz ◽  
Tibor Sabo
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Nmr Spectra ◽  
Symmetry Axis ◽  
Layer Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

A new R2edda-type ester, diisobutyl (S,S)-2,2'-(1,2-ethane-diyldiimino) di(4-methylpentanoate) dihydrochloride, [(S,S)-H2iBu2eddl]Cl2, 1, and its palladium(II) complex, dichloro(diisobutyl (S,S)-2,2'-(1,2-ethanediyldiimino) di(4-methylpentanoate))palladium(II), [PdCl2{(S,S)-iBu2eddl}], 2, were synthesized and characterized by elemental analysis, as well as IR and NMR spectroscopy. It was found that complex 2 was obtained as mixture of two diastereoisomers, observed in NMR spectra. The crystal structure of compound 1 was determined by X-ray diffraction studies and is described. The isolated crystals consisted of one dicationic species [(S,S)-H2iBu2eddl]2+ and two Cl-. The crystal system was tetragonal with the space group P42. Hydrogen bonds significant for the manner of packing are N-H1N???Cl, 3.049(3) ?, 159(3)? and N-H2N???Cl, 3.100(3) ?, 164(3)?. An infinite chain was formed building a one layer structure, usual for these types of compounds. The C2 symmetry axis of the compound passes through the C1-C1i bond vector and lies perpendicular to the plane N2Cl2.

Synthese und Charakterisierung von Halogen-phosphor(III)- Derivaten des 8-Hydroxychinolins. Röntgenstrukturanalyse von 8-[Phenyl(chloro)-phosphito]-chinolin/ Synthesis and Characterization of Halogen-phosphorus(III) Derivatives of 8-Hydroxyquinoline. X -Ray Structure Analysis of 8-[Phenyl(chloro)phosphito]-quinoline

1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds ◽  
Derivatives Of

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.

Synthesis and Characterization of 3-Chloropropyl-substituted o- Carboranes: Crystal Structures of 1,2-(1,3-Propanediyl)-o-carborane, 1-(3-Chloropropyl)-o-carborane and 1,2-Bis(3-chloropropyl)-ocarborane

2013 ◽  
Vol 68 (7) ◽  
pp. 804-810 ◽  
Author(s):  
Deqian Bian ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Ping Lu
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Main Product ◽  
Total Yield ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reactions of the lithio-o-carborane Li2C2B10H10 with ClCH2CH2CH2Br were studied under various conditions. While the main product is the known exo-polyhedrally cyclized 1,2- (1,3-propanediyl)-o-carborane (2), the expected 3-chloropropyl-substituted carborane products 1- (ClCH2CH2CH2)C2B10H11 (3) and 1,2-(ClCH2CH2CH2)2C2B10H10 (4) can be obtained in a total yield of 22%. In the presence of CuCl, the same reaction proceeded rather slowly and gave compound 3and bis(o-carborane) (5) in small yields, with the recovery of the starting o-C2B10H12. Compounds 2- 4were characterized by means of IR and NMR spectroscopy and mass spectrometry, as well as by single-crystal X-ray diffraction.

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