scholarly journals  Preparation of N-alkylamides of highly methylated (HM) citrus pectin

2011 ◽  
Vol 21 (No. 5) ◽  
pp. 162-166 ◽  
Author(s):  
A. Syntsya ◽  
J. Čpíková ◽  
M. Marounek ◽  
P. Mlčochová ◽  
L. Sihelková ◽  
...  

N-Alkylamides of highly methylated (HM) citrus pectin (DM = 73%) were prepared using heterogeneous amino-de-alkoxylation (aminolysis) with five selected n-alkylamines. The reaction was carried out in N,N-dimethylformamide at 8&deg;C (n-butylamine), 25&deg;C (n-hexylamine), and 45&deg;C (n-octylamine, n-dodecylamine and n-octadecylamine). All the derivatives were converted into acid forms by washing with acidic water-ethanol mixture. The products were analysed by organic elemental analysis, diffusion reflection FT-IR spectroscopy and by 13C CP/MAS NMR. Both FT-IR and NMR spectra indicate the presence of alkylamide substituents bound to pectin. The degrees of amidation (DA) of the derivatives and molar and mass reaction yields (Y<sub>m</sub>and Y<sub>n</sub>) were calculated based on the results of elemental analysis. The DA values of the N-alkylamides were 39&ndash;55% that corresponded to Y<sub>n</sub>of 54&ndash;75%. &nbsp;

2016 ◽  
Vol 71 (1) ◽  
pp. 81-84 ◽  
Author(s):  
Eugen Weisheim ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.


2020 ◽  
Vol 76 (7) ◽  
pp. 690-694
Author(s):  
Qianjun Deng ◽  
Jiming Wang ◽  
Guangzhao Li ◽  
Shuhua Zhang

A new ionic pentanuclear FeIII cluster, namely, triethylazanium tetrakis(μ2-5-amino-1,2,3,4-tetrazolido)tetrakis(μ3-4-chloro-2-{[(1H-tetrazol-1-id-5-yl)imino]methyl}phenolato)di-μ3-oxido-pentairon(III) acetonitrile monosolvate monohydrate, (C6H16N)[Fe5(C8H4ClN5O)4(CH2N5)4O2]·CH3CN·H2O, was synthesized using microvial synthesis methods and characterized by elemental analysis, FT–IR spectroscopy, single-crystal X-ray diffraction and thermogravimetric analysis. Magnetic studies reveal that the complex displays dominant antiferromagnetic intracluster interactions between the FeIII ions through the μ3-oxide bridges.


2013 ◽  
Vol 750-752 ◽  
pp. 1750-1753
Author(s):  
Rui Jia ◽  
Hai Yan Xu ◽  
Qi Feng ◽  
Wen Bao Li ◽  
Bao Hua Zhu

Four new arylamine-acetylene bridged tetrahedral iron and cobalt carbonyl clusters, [Co2(CO)4(μ-CO)2(η2, μ-TMSCCPh)2N 1, [Fe2(CO)6(μ-CO)(η2, μ-TMSCCPh)NH(PhCC TMS)] 2, [(Co2(CO)6(η2, μ-TMSCCPh))33 and [(Fe2(CO)6(μ-CO)(η2, μ-TMSCCPh))2N(Ph CCTMS)] 4, were obtained by reactions of Co2(CO)8and Fe3(CO)12with the bis [4-((trimethylsilyl) ethynyl) phenyamine and tris [4-((trimethylsilyl) ethynyl) phenyamine compounds in suitable solvent, respectively. All clusters are confirmed by C/H elemental analysis, MS,1HNMR and FT-IR spectroscopy. Furthermore, the electrochemical and optical properties of some clusters were also determined by cyclic voltammogram (CV) analysis and UV-Vis spectra.


2010 ◽  
Vol 63 (2) ◽  
pp. 252 ◽  
Author(s):  
Jingli Xie ◽  
Ryan Gilbert-Wilson ◽  
Boujemaa Moubaraki ◽  
Keith S. Murray ◽  
Anthony G. Wedd

Two new hybrid materials [Fe(bipy)3]3[ZnW12O39(OH)Fe(bipy)2(H2O)]2 and [Fe(bipy)3]2[CoW12O40] were obtained by hydrothermal synthesis. They contain [Fe(bipy)3] n+ (bipy = 2,2′-bipyridyl; n = 2 or 3) cations and Keggin-type polyoxotungstate anions. Both have been characterized by elemental analysis, FT-IR spectroscopy, 1H-NMR spectrometry, and single crystal X-ray crystallography. The anion in the former salt features [FeII(bipy)2(OH2)]2+ units covalently bound via a W=O-Fe bridge to the protonated anion [ZnW12O39(OH)]5–. The latter salt contains discrete [CoW12O40]6– anions.


1999 ◽  
Vol 09 (03n04) ◽  
pp. 465-473
Author(s):  
N. KAGEMORI ◽  
K. UMEMURA ◽  
T. YOSHIMURA ◽  
M. INOUE ◽  
S. KAWAI ◽  
...  

Six types of samples including urushi, urushi tree and black coating films taken from ancient Buddha images were examined by analyses of PIXE, organic element and FT-IR to identify with urushi another material. Based on the results of three analytical experiments above mentioned, the coating materials aging over hundreds of years were identified with weathered urushi films mixed with other material. Further investigation may reveal the urushi coating techniques used in the past.


2012 ◽  
Vol 6 (1) ◽  
pp. 28-33 ◽  
Author(s):  
Xin Xing ◽  
Aiqing Gguo ◽  
Lin Liu ◽  
Xiaodong Li

Novel polysilanes, antimony-substituted polysilanes (APS) and iron-substituted polysilanes (IPS), were synthesized and characterized in this paper. To prepare these new metal-containing polymers, high reactive polymers, polymethylsilane (PMS) and polychloromethylsilane (PCMS) were used as mother polymers. The APS was synthesized directly by the reaction of PMS with SbCl3, while IPS was obtained from the reaction of PCMS with Na2Fe(CO)4 in the solvent of n-hexane. The polymers were characterized by elemental analysis, FT-IR, 1H-NMR, 29Si CP/MAS NMR, GPC, and UV. The number average molecular weights of these two polymers are between 1400 and 1600. These polymers show good semiconductive properties, whose intrinsic conductivities are in the range of 10-8~10-7S/cm, and can be increased to10-5S/cm after being doped with iodine.


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