Les oxazolines-4 précurseurs de sels d'iminium fonctionnels. Ouverture en milieu anhydre de ces hétérocycles par des acides protoniques: obtention de sels d'iminium fonctionnels, étude de leur structure

1979 ◽  
Vol 57 (21) ◽  
pp. 2876-2884 ◽  
Author(s):  
Michel Vaultier ◽  
Gurbachan Mullick ◽  
Robert Carrié

The protonation of 4-oxazolines with protic acids in anhydrous medium, both at low or at room temperature, generally leads to acyclic functional iminium salts. In those cases where the oxazoline ring bears a hydrogen atom in the four position, two diastereoisomeric cyclic iminium salts are obtained. The conditions for preparation of these salts along with the characterization of their structures were determined by the aid of 1H and 13C nmr.

1982 ◽  
Vol 60 (18) ◽  
pp. 2372-2382 ◽  
Author(s):  
R. H. Marchessault ◽  
Suzanne Coulombe ◽  
Hiromichi Morikawa ◽  
Danielle Robert

Exploded wood lignin (EXWL) was extracted from moist steam hydrolysed aspen (Populustremuloides) wood using methanol. The lignin was examined by elemental analysis, gel permeation chromatography, infrared spectroscopy, proton and 13C nmr. The observed nmr spectra were compared with those of aspen milled wood lignin (MWL). Typical composition of the material is C9H9.2O2.7(OCH3)1.1 Assignment of all the signals in the nmr spectrum led to the conclusion that the explosion process causes cleavage of the β-aryl-ether bond. The weight average molecular weight was found to be 1700–1900 and the polydispersity 2.6. The finely divided exploded wood was soluble in 90% methanol/water mixtures to well beyond 20% by weight at room temperature.


2013 ◽  
Vol 68 (5-6) ◽  
pp. 598-604 ◽  
Author(s):  
Shuang Yue ◽  
Da-Wei Fang ◽  
Jun Li ◽  
Shu-Liang Zang ◽  
Ming-Dong Zhou ◽  
...  

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


Author(s):  
Bradley L. Thiel ◽  
Chan Han R. P. ◽  
Kurosky L. C. Hutter ◽  
I. A. Aksay ◽  
Mehmet Sarikaya

The identification of extraneous phases is important in understanding of high Tc superconducting oxides. The spectroscopic techniques commonly used in determining the origin of superconductivity (such as RAMAN, XPS, AES, and EXAFS) are surface-sensitive. Hence a grain boundary phase several nanometers thick could produce irrelevant spectroscopic results and cause erroneous conclusions. The intergranular phases present a major technological consideration for practical applications. In this communication we report the identification of a Cu2O grain boundary phase which forms during the sintering of YBa2Cu3O7-x (1:2:3 compound).Samples are prepared using a mixture of Y2O3. CuO, and BaO2 powders dispersed in ethanol for complete mixing. The pellets pressed at 20,000 psi are heated to 950°C at a rate of 5°C per min, held for 1 hr, and cooled at 1°C per min to room temperature. The samples show a Tc of 91K with a transition width of 2K. In order to prevent damage, a low temperature stage is used in milling to prepare thin foils which are then observed, using a liquid nitrogen holder, in a Philips 430T at 300 kV.


1999 ◽  
Vol 64 (6) ◽  
pp. 977-985 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Hans-Jörg Schanz ◽  
Wolfgang Milius ◽  
Catherine McCammon

Sodium hexaethyl-2,4-dicarba-nido-hexaborate(1-) (6), available from hexaethyl-2,4-dicarba- nido-hexaborane(8) (4) by deprotonation, reacts with deuterated methanol, CD3OD, to give back 4 without H/D exchange of the B-H-B hydrogen atom. The reaction of 6 with diethylboron chloride, Et2BCl, affords hexaethyl-2,4-dicarba-closo-hexaborane(6) (7), the first example of a peralkylated carborane of this type. In contrast, the reaction of 6 with boron tribromide, BBr3, leads mainly to 2,3,4,5,6,7-hexaethyl-2,4-dicarba-closo-heptaborane(7) (8), together with the corresponding 1-bromo derivative (9) and the closo-carborane 7 as side products. The reaction of two equivalents of 6 with FeCl2 gives the air-stable sandwich complex bis[hexaethyl-2,4-dicarba-nido-hexaborate(1-)]iron 10 which was characterised by X-ray structural analysis. All products were characterised by 1H, 11B and 13C NMR spectroscopy, and 57Fe Mössbauer spectroscopy was used to study 10.


2020 ◽  
Vol 74 (11) ◽  
pp. 866-870
Author(s):  
Lewis C. H. Maddock ◽  
Alan Kennedy ◽  
Eva Hevia

While fluoroaryl fragments are ubiquitous in many pharmaceuticals, the deprotonation of fluoroarenes using organolithium bases constitutes an important challenge in polar organometallic chemistry. This has been widely attributed to the low stability of the in situ generated aryl lithium intermediates that even at –78 °C can undergo unwanted side reactions. Herein, pairing lithium amide LiHMDS (HMDS = N{SiMe3}2) with FeII(HMDS)2 enables the selective deprotonation at room temperature of pentafluorobenzene and 1,3,5-trifluorobenzene via the mixed-metal base [(dioxane)LiFe(HMDS)3] (1) (dioxane = 1,4-dioxane). Structural elucidation of the organometallic intermediates [(dioxane)Li(HMDS)2Fe(ArF)] (ArF = C6F5, 2; 1,3,5-F3-C6H2, 3) prior electrophilic interception demonstrates that these deprotonations are actually ferrations, with Fe occupying the position previously filled by a hydrogen atom. Notwithstanding, the presence of lithium is essential for the reactions to take place as Fe II (HMDS)2 on its own is completely inert towards the metallation of these substrates. Interestingly 2 and 3 are thermally stable and they do not undergo benzyne formation via LiF elimination.


RSC Advances ◽  
2021 ◽  
Vol 11 (22) ◽  
pp. 13245-13255
Author(s):  
Mehdi Davoodi ◽  
Fatemeh Davar ◽  
Mohammad R. Rezayat ◽  
Mohammad T. Jafari ◽  
Mehdi Bazarganipour ◽  
...  

New nanocomposite of zeolitic imidazolate framework-67@magnesium aluminate spinel (ZIF-67@MgAl2O4) has been fabricated by a simple method at room temperature with different weight ratios.


2010 ◽  
Vol 75 ◽  
pp. 202-207
Author(s):  
Victor Ríos ◽  
Elvia Díaz-Valdés ◽  
Jorge Ricardo Aguilar ◽  
T.G. Kryshtab ◽  
Ciro Falcony

Bi-Pb-Sr-Ca-Cu-O (BPSCCO) and Bi-Pb-Sb-Sr-Ca-Cu-O (BPSSCCO) thin films were grown on MgO single crystal substrates by pulsed laser deposition. The deposition was carried out at room temperature during 90 minutes. A Nd:YAG excimer laser ( = 355 nm) with a 2 J/pulse energy density operated at 30 Hz was used. The distance between the target and substrate was kept constant at 4,5 cm. Nominal composition of the targets was Bi1,6Pb0,4Sr2Ca2Cu3O and Bi1,6Pb0,4Sb0,1Sr2Ca2Cu3OSuperconducting targets were prepared following a state solid reaction. As-grown films were annealed at different conditions. As-grown and annealed films were characterized by XRD, FTIR, and SEM. The films were prepared applying an experimental design. The relationship among deposition parameters and their effect on the formation of superconducting Bi-system crystalline phases was studied.


Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3502
Author(s):  
Fangzhou Song ◽  
Masayoshi Uematsu ◽  
Takeshi Yabutsuka ◽  
Takeshi Yao ◽  
Shigeomi Takai

LATP-based composite electrolytes were prepared by sintering the mixtures of LATP precursor and La2O3 nano-powder. Powder X-ray diffraction and scanning electron microscopy suggest that La2O3 can react with LATP during sintering to form fine LaPO4 particles that are dispersed in the LATP matrix. The room temperature conductivity initially increases with La2O3 nano-powder addition showing the maximum of 0.69 mS∙cm−1 at 6 wt.%, above which, conductivity decreases with the introduction of La2O3. The activation energy of conductivity is not largely varied with the La2O3 content, suggesting that the conduction mechanism is essentially preserved despite LaPO4 dispersion. In comparison with the previously reported LATP-LLTO system, although some unidentified impurity slightly reduces the conductivity maximum, the fine dispersion of LaPO4 particles can be achieved in the LATP–La2O3 system.


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