scholarly journals Synthesis and properties of novel ammonium-based room-temperature gemini ionic liquids

RSC Advances ◽  
2018 ◽  
Vol 8 (46) ◽  
pp. 26255-26265 ◽  
Author(s):  
Xuzhao Yang ◽  
Yun Fang
Keyword(s):  
Ionic Liquids ◽  
Room Temperature ◽  
H Nmr ◽  
C Nmr

Ammonium-based asymmetrical gemini ionic liquids, 1-trimethylammonium-3-(pyridinium)propane bisdicyanamide and 1-trimethylammonium-3-(1-methylpiperidinium)propane bisdicyanamide were respectively synthesized and characterized by 1H NMR and 13C NMR.

scholarly journals New Method for Nucleophilic Substitution on Hexachlorocyclotriphosphazene by Allylamine Using an Algerian Proton Exchanged Montmorillonite Clay (Maghnite-H+) as a Green Solid Catalyst

2016 ◽  
Vol 11 (2) ◽  
pp. 151 ◽  
Author(s):  
Lahouaria Medjdoub ◽  
Belbachir Mohammed
Keyword(s):  
Nucleophilic Substitution ◽  
Room Temperature ◽  
Montmorillonite Clay ◽  
New Method ◽  
Solid Catalyst ◽  
H Nmr ◽  
Flight Mass Spectrometry ◽  
Crystalline Product ◽  
First Time ◽  
C Nmr

<p>Nucleophilic substitution on hexachlorocyclotriphosphazene (HCCTP) with allylamine in order to give hexa(allylamino)cyclotriphosphazene (HACTP)  is performed for the first time under mild conditions by using diethylether as solvent to replace benzene which is very toxic. The reaction time is reduced to half and also performed at room temperature but especially in the presence of an eco-catalyst called Maghnite-H<sup>+</sup>. This catalyst has a significant role in the industrial scale. In fact, the use of Maghnite is preferred for its many advantages: a very low purchase price compared to other catalysts, the easy removal of the reaction mixture. Then, Maghnite-H<sup>+</sup> is became an excellent catalyst for many chemical reactions. The structure of HACTP synthesized in the presence of Maghnite-H<sup>+</sup> to 5% by weight is confirmed by <sup>1</sup>H-NMR, <sup>13</sup>C-NMR, <sup>31</sup>P-NMR (Nuclear magnetic resonance) and FTIR (Fourier Transform Infrared spectroscopy). MALDI-TOF (Matrix-Assisted Laser Desorption/Ionisation-time-of-flight mass spectrometry) is used to establish the molecular weight of HACTP which is 471 g/mol. DSC (Differential Scanning Calorimetery) and TGA (Thermogravimetric Analysis) show that HACTP is a crystalline product with a melting point of 88 °C. It is reactive after melting but is degraded from 230 °C. Copyright © 2016 BCREC GROUP. All rights reserved</p><p><em>Received: 28<sup>th</sup> September 2015; Revised: 5<sup>th</sup> December 2015; Accepted: 4<sup>th</sup> January 2016</em></p><p><strong>How to Cite</strong>: Medjdoub, L., Mohammed, B. (2016). New Method for Nucleophilic Substitution on Hexachlorocyclotriphosphazene by Allylamine Using an Algerian Proton Exchanged Montmorillonite Clay (Maghnite-H+) as a Green Solid Catalyst. <em>Bulletin of Chemical Reaction Engineering &amp; Catalysis</em>, 11 (2): 151-160 (doi:10.9767/bcrec.11.2.541.151-160)</p><p><strong>Permalink/DOI:</strong> http://dx.doi.org/10.9767/bcrec.11.2.541.151-160</p>

Metall-π-Komplexe yon Benzolderivaten, XIII Bis(methylthio-η-beiizol)chrom(0) Darstellung und Einsatz als zweizähniger Chelatligand/ Metal-π Complexes of Benzene Derivatives, XIII Bis(methylthio-η-benzene)chromium(0) Preparation and Function as a Bidentate Chelating Ligand

1981 ◽  
Vol 36 (1) ◽  
pp. 94-101 ◽  
Author(s):  
Helmut Burdorf ◽  
Christoph Eischenbroich
Keyword(s):  
Nmr Spectra ◽  
Room Temperature ◽  
Radical Cations ◽  
Esr Spectra ◽  
Benzene Derivatives ◽  
Consecutive Reaction ◽  
H Nmr ◽  
Chelating Ligand ◽  
And Function ◽  
C Nmr

Abstract The thioanisole-π-complexes (methylthio-η-benzene)-(η-benzene)-chromium (2) and bis(methylthio-η-benzene)chromium (3) have been prepared via lithiation of bis(η-benzene)-chromium and consecutive reaction with dimethyldisulfide. 1H NMR and 13C NMR spectra of 2 and 3 as well as ESR-spectra of the corresponding radical cations 2.+ and 3.+ were recorded and analyzed. In contrast to C(η-arene)-Si and C(η-arene)-P bonds, C(y-arene)-S bonds are stable to solvolysis. With (norbornadiene)tetracarbonylmolybdenum, 3 readily forms [bis(methylthio-η-benzene)chromium]tetracarbonylmolybdenum (6) wherein 3 functions as a chelating ligand. 1H and 13C NMR evidence suggests, that at room temperature 6 undergoes rapid conformational interconversions.

Chemical stability of CVD source materials for high-Tc superconducting films

1992 ◽  
Vol 7 (6) ◽  
pp. 1336-1340 ◽  
Author(s):  
Takuya Hashimoto ◽  
Hideomi Koinuma ◽  
Masaaki Nakabayashi ◽  
Tadashi Shiraishi ◽  
Youichi Suemune ◽  
...  
Keyword(s):  
Chemical Stability ◽  
Room Temperature ◽  
Chemical Vapor ◽  
Superconducting Films ◽  
Adsorbed Species ◽  
High Tc ◽  
H Nmr ◽  
The Stability ◽  
Source Materials ◽  
C Nmr

The stability of chemical vapor deposition (CVD) source materials for high-Tc superconducting films was examined by 1H-NMR (nuclear magnetic resonance), 13C-NMR, IR (infrared) absorption, and TG-DTA (thermogravimetry and differential thermal analysis) measurements. Highly purified Ca(DPM)2 (DPM: dipyvaloylmethane: (CH3)3CCOCHCOC(CH3)3) and Sr(DPM)2, utilizing recrystallization and sublimation, easily decomposed at room temperature and changed their thermal properties when they were handled and stored in air or even in an Ar atmosphere without removing adsorbed species such as water. The stability increased by removing a trace of adsorbed species and storing in an Ar atmosphere at −30 °C. Bi(C6H5)3 and Y(DPM)3 showed higher chemical stability than Ca(DPM)2 and Sr(DPM)2.

1,4-Bis(p-pentazolylphenyl)butan, 1-p-Azidophenyl-4-p-pentazolylphenyl- butan und 1,4-Bis(p-azidophenyl)butan / 1,4-Bis(p-pentazolylphenyl)butane, 1-p-Azidophenyl-4-p-pentazolylphenyl-butane and 1,4-Bis(p-azidophenyl)butane

2004 ◽  
Vol 59 (6) ◽  
pp. 716-720 ◽  
Author(s):  
Frank Biesemeier ◽  
Klaus Harms ◽  
Ulrich Müller
Keyword(s):  
Low Temperature ◽  
Sodium Azide ◽  
Rate Constants ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Fine Powder ◽  
Space Group ◽  
H Nmr ◽  
Diazonium Ions ◽  
C Nmr

1,4-Bis(p-pentazolylphenyl)butane (1), 1-p-azidophenyl-4-p-pentazolylphenyl-butane (2) and 1,4-bis(p-azidophenyl)butane (3) were obtained by the reaction of 1,4-diphenylbutane-4’,4”- bis(diazonium) ions with sodium azide in methanol at −50 °C. In the 1H and 13C NMR spectra the three compounds can be distinguished unequivocally. At −50 °C a mixture with a composition 1:2:3 of 10:30:60 was obtained. By recrystallization first from dichloromethane/methanol and then from dichloromethane/petroleum ether the pentazole components were enriched to a composition ratio of 21:62:17. The rate constants of the decompositions 1→2 and 2→3 at 0 °C were determined from the variation of the 1H NMR intensities. At room temperature all of the material is converted to 3. 3 crystallizes in two monoclinic modifications. At −70 °C a modification 3-LT having space group P21/c (a = 950.8, b = 1192.6, c = 701.3 pm, β = 92.55°, Z = 2; R = 0.075) was obtained. The modification crystallizing at room temperature (3-HT) has space group I2/a (a = 1514.5, b = 498.1, c = 2027.9 pm, β = 92.73°, Z = 4; R = 0.040). Whereas both modifications consist of nearly identical molecules, their packings are quite different. When the low temperature modification is warmed to room temperature, its crystals jump like flees and are disrupted to a fine powder.

scholarly journals A novel hyperbranched polyester based on 2,2-bis(hydro xylmethyl)butyric acid: synthesis and characterization

e-Polymers ◽  
2007 ◽  
Vol 7 (1) ◽  
Author(s):  
Michelina Soccio ◽  
Lara Finelli ◽  
Nadia Lotti ◽  
Paola Marchese ◽  
Valentina Siracusa ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Butyric Acid ◽  
Room Temperature ◽  
Cyanuric Acid ◽  
Acid Synthesis ◽  
Hyperbranched Polyester ◽  
Degree Of Branching ◽  
Good Thermal Stability ◽  
H Nmr ◽  
C Nmr

AbstractA novel hyperbranched polyester was synthesized in bulk from 2,2- bis(hydroxymethyl)butyric acid and two different core molecules (1,1,1-tris- (hydroxylmethyl)propane and 1,3,5-tris(2-hydroxyethyl)cyanuric acid), using ptoluensolfonic acid, scandium trifluoromethanesulfonate, titanium tetrabutoxide and dibutyltin oxide as catalysts and varied reaction temperature and time. At room temperature the samples obtained appeared as glassy, slightly yellow solids, with Mn (calculated by 1H-NMR spectra) in the range 500 - 2000. The degree of branching of the polyesters was determined by 13C-NMR spectroscopy and was found in the range 0.32 - 0.53. The introduction of the monomer in various steps seems to influence slightly the degree of branching, but has no effect on the molecular weight of these polymers. The polyesters exhibited a good thermal stability, as revealed by TGA technique, and the glass transition temperature, determined by DSC, was found to depend on the molecular weight and the kind of catalyst employed.

scholarly journals NMR and Mass Spectroscopic Studies on Catharine

1985 ◽  
Vol 40 (4) ◽  
pp. 543-545 ◽  
Author(s):  
◽  
Irshad Ali ◽  
M. Iqbal Chaudhary
Keyword(s):  
Room Temperature ◽  
Spectroscopic Studies ◽  
Temperature Dependent ◽  
Mass Spectral Fragmentation ◽  
Mass Spectral ◽  
H Nmr ◽  
Temperature Dependent Study ◽  
C Nmr

The 13C NMR of Catharine is reported. A temperature-dependent study of the 1H NMR of Catharine indicates that it exists as two conformers at room temperature. At higher temperatures, the distinction between the two conformers disappears with the higher rate of equilibration. The mass spectral fragmentation of Catharine as established by link scan measurements is also re­ported.

Synthesis of 3,4-Disubstituted Poly(thiophene)s via Substitution of Poly(3-alkylthiophene)

2001 ◽  
Vol 665 ◽  
Author(s):  
Yuning Li ◽  
George Vamvounis ◽  
Steven Holdcroft
Keyword(s):  
Electrophilic Substitution ◽  
Room Temperature ◽  
Bromine Atom ◽  
Side Chain ◽  
Hydrogen Atoms ◽  
H Nmr ◽  
Regioregular Poly ◽  
Fuming Nitric Acid ◽  
Preliminary Study ◽  
C Nmr

ABSTRACTThe electrophilic substitution of regioregular poly(3-hexylthiophene) (P3HT) at the 4- position was investigated to produce structurally well defined 3,4-disubstituted poly(thiophene)s. When P3HT was treated with N-bromosuccinimide (NBS) in chloroform at 25 to 50 °C, the 4-hydrogen atom in P3HT is completely substituted by bromine, as indicated by the 1H NMR, 13C NMR and elemental analysis. Similarly, the chlorinated product was obtained using N- chlorosuccinimide (NCS) at room temperature. However, only 85% of the 4-hydrogen atoms were replaced by chlorine and ∼15% of the α-hydrogen atoms on the hexyl side chain were chlorinated. P3HT readily reacts with fuming nitric acid in chloroform at 0 °C to generate a nitrated product with almost 100% substitution at the 4-position. Our preliminary study on the futher functionalizaton of these polymers was conducted on the brominated product. Our results showed that the bromine atom in this polymer could be further substituted with other groups.

Synthesis and Characterization of Imidazolium Perrhenate Ionic Liquids

2013 ◽  
Vol 68 (5-6) ◽  
pp. 598-604 ◽  
Author(s):  
Shuang Yue ◽  
Da-Wei Fang ◽  
Jun Li ◽  
Shu-Liang Zang ◽  
Ming-Dong Zhou ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Ionic Liquids ◽  
Room Temperature ◽  
Alkyl Chain ◽  
Alkyl Chain Length ◽  
Synthesis And Characterization ◽  
Room Temperature Ionic Liquids ◽  
Ionization Mass ◽  
C Nmr

A series of air- and water-stable imidazolium perrhenate-based room-temperature ionic liquids [(RT)ILs] of the type [Cnmim][ReO4] (Cnmim = 1-CnH2n+1-3-methylimidazolium, n = 2, 4, 5, 6, 8, 10, 12) have been synthesized and characterized by 1H and 13C NMR spectroscopy, IR spectroscopy, electrospray ionization mass spectrometry (ESI-MS), and elemental analysis (EA). The effect of the variation of the alkyl chain length on physical properties such as melting point, thermal stability, density, and conductivity was examined

scholarly journals Room temperature ionic liquids based on cationic porphyrin derivatives and tetrakis(pentafluorophenyl)borate anion

2011 ◽  
Vol 15 (07n08) ◽  
pp. 560-574 ◽  
Author(s):  
Hai-Jun Xu ◽  
Claude P. Gros ◽  
Stéphane Brandès ◽  
Pei-Yu Ge ◽  
Hubert H. Girault ◽  
...  
Keyword(s):  
Ionic Liquids ◽  
Room Temperature ◽  
Specific Conductivity ◽  
Counter Anion ◽  
Visible Spectroscopy ◽  
Cationic Porphyrin ◽  
H Nmr ◽  
Porphyrin Derivatives ◽  
Uv Visible ◽  
High Yields

A series of 11 low melting ionic liquids based on meso-substituted A3B -porphyrins and A2B2-porphyrins containing one or two pyridyl substituents have been synthesized in high yields. Three of them are liquids at room temperature. All these porphyrinic salts were characterized by1H NMR,19F NMR, MALDI-TOF mass spectrometry, elemental analysis and UV-visible spectroscopy. The thermal properties and conductivity values of these salt derivatives have been also measured. A specific conductivity value of up to 4 mS.cm-1could be obtained for a compound having the counter-anion B(C6F5)4-.

Physicochemical properties of novel cholinium ionic liquids for the recovery of silver from nitrate media

RSC Advances ◽  
2015 ◽  
Vol 5 (95) ◽  
pp. 78268-78277 ◽  
Author(s):  
Rafael M. Rios-Vera ◽  
Juliette Sirieix-Plénet ◽  
Laurent Gaillon ◽  
Cécile Rizzi ◽  
Mario Ávila-Rodríguez ◽  
...  
Keyword(s):  
Ionic Liquids ◽  
Physicochemical Properties ◽  
Esi Ms ◽  
H Nmr ◽  
Extraction Properties ◽  
C Nmr

Linear and ramified cholinium based ionic liquids have been synthesized and their physicochemical properties have been investigated by 1H NMR, 13C NMR, ATR-FTIR and ESI-MS as well as their extraction properties towards Ag(i), Cu(ii) and Fe(iii).

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