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1.
2.
Mark Edgar Dee Hayward Fatemeh Zeinali Shahzad Riaz George W. Weaver 《Magnetic resonance in chemistry : MRC》2020,58(2):170-185
A simple to use nuclear magnetic resonance analysis method has been tested on complex 1H, 19F, and 13C multiplets. This open-source line-shape analysis method analysis of total lineshape (ANATOLIA)1 provides some significant advantages over traditional assign-iterate methods of NMR spectral analysis by avoiding false minima and progressing optimisation to the global minimum. The target molecules are 1-perfluorotol-4-yl-2-perfluorotol-4-yl-oxymethyl-1H-benzimidazole (molecule-I) and 1-tetrafluoropyrid-4-yl-2-tetrafluoropyrid-4-yl-thio-1H-benzimidazole (molecule-II) which were produced as part of a family of fluorinated drug scaffolds prepared for anticancer and antiparasitic screening. Spectra display significant second-order effects with 1H Δδ = 3.68 and 4.67 Hz for the aromatic hydrogen “triplets”, with 19F 4JAA', 4JBB', 4JXX', and 4JYY' coupling constants range from +4.8 to −14.0 Hz and for 13C-isotopomers 19F Δδ of up to 111.56 Hz. A spin-system of six coupling nuclei (HaHbHcHd FYFY') was analysed in 12 s, a spin-system of nine coupling fluorine nuclei (AA'BB'CCC-YY') was analysed within 2 min, and 10 coupling nuclei (XX'YY'ZZZ-BB'-Hd) was optimised in 6 min using a laptop computer. ANATOLIA was also robust enough to be able to yield accurate spectral values from inaccurate input values. In both compounds, a fluorine–fluorine coupling constant was identified between the two fluoro-aromatic rings (FBB' and FYY') of +4.05 and +4.67 Hz and attributed to a through-space interaction. Ab initio structure optimisations and coupling constant calculations provided useful input data for spectral analysis. A modern 19F nuclear magnetic resonance spectrum of perfluorotoluene (octafluorotoluene) and analysis from 1975 was used as a test data set to assess ANATOLIA. 相似文献
3.
Najmedin Azizi 《Tetrahedron letters》2004,45(50):9233-9236
Under solvent-free reaction conditions and in the presence of solid LiClO4 a novel and mild protocol for the one-pot, three-component synthesis of primary α-amino phosphonates from an aldehyde, hexamethyldisilazane and a trialkyl phosphite is described giving high yields and having short reaction times. The same products are obtained in very low yields, when the three-component reaction is carried out under microwave irradiation and in the absence of solid LiClO4. Examples of some prepared 1-aryl-N,N′-bis(arylidene)methanediamines are also described. 相似文献
4.
Treatment of aliphatic and aromatic aldehydes with chiral amines and trimethylsilyl cyanide in the absence or in the presence
of Lewis acids (including lithium perchlorate) under solvent-free conditions afforded the corresponding α-aminonitriles in
good yields and with a diastereoselectivity of 68 to 86%.
Published in Russian in Zhurnal Organicheskoi Khimii, 2006, Vol. 42, No. 1, pp. 56–59.
The text was submitted by the authors in English. 相似文献
5.
Harris RK Kinnear KA Morris GA Stchedroff MJ Samadi-Maybodi A Azizi N 《Chemical communications (Cambridge, England)》2001,(23):2422-2423
The first use of silicon-29 diffusion-ordered NMR spectroscopy (DOSY) is reported, in a study of the speciation of aqueous silicates. 相似文献
6.
J. A. Azizi D. Dollimore P. J. Dollimore G. R. Heal P. Manley W. A. Kneller W. Jin Yong 《Journal of Thermal Analysis and Calorimetry》1993,40(2):831-847
In this study a relationship between the surface and textural properties of carbon blacks and the gasification process induced thermally in air is noted. A temperature jump method was used to follow the gasification in air and to establish the relevant Arrhenius parameters. This can be associated with the activity of ‘basal’ plane carbon atoms as well as ‘edge’ carbon atoms at the surface. This is based on a model of carbon black structure consisting of the irregular packing of small graphite carbon structures. The carbon black surface was measured using a single measurement of adsorption based essentially on the BET volumetric method. The carbon black surface had a rate of oxidation per unit are which clearly indicated that the lower area carbon blacks had a predominately active area of ‘edge’ atoms at the surface while the surface of the higher area carbon blacks had a predominate amount of ‘basal’ plane graphite carbon atoms. 相似文献
7.
Arab Chamjangali M Bagherian G Azizi G 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2005,62(1-3):189-196
A simple, novel and sensitive spectrophotometric method was described for the simultaneous determination of cobalt, nickel and palladium. The method is based on the complex formation of Co, Ni and Pd with 1-(2-pyridylazo)-2-naphtol (PAN) in Tween-80 micellar media. All factors affecting on the sensitivity were optimized and the linear dynamic range for determination of Co, Ni and Pd was found. The experimental calibration matrix was designed by measuring the absorbance over the range of 520-700 nm for 21 samples of 0.10-1.0, 0.050-0.50 and 0.050-4.0 microg ml(-1) of Co, Ni and Pd, respectively. The partial least square (PLS) modeling based on singular value decomposition (SVD) was used for the multivariate calibration of the spectrophotometric data. The direct orthogonal signal correction was used for pre-processing of data matrices and the prediction results of model, with and without using direct orthogonal signal correction, were statistically compared. The effects of various anions and cations on selectivity of the method were investigated. The proposed method was successfully applied to the determination of Co, Ni and Pd in water and alloy samples. 相似文献
8.
Mohammad Ali Zolfigol Iraj Mohammadpoor-BaltorkDavood Habibi BiBi Fatemeh MirjaliliAbdolhamid Bamoniri 《Tetrahedron letters》2003,44(44):8165-8167
Primary and secondary trimethylsilyl ethers were converted to their corresponding ethers in the presence Nafion-H® with good to excellent yields under mild and heterogeneous conditions. 相似文献
9.
10.
Stephen E. Ullrich Esther Azizi Margaret L. Kripke 《Photochemistry and photobiology》1986,43(6):633-638
Abstract— After a single exposure of mice to UV radiation, their ability to generate a contact hypersensitivity (CHS) response to contact sensitizers applied epicutaneously to distant, unirradiated skin is severely impaired. It is not clear, however, if the classic delayed type hypersensitivity (DTH) reponse to exogenous antigens, injected into the subcutaneous (s.c.) space, can also be modulated by UV radiation. We report here that a single exposure of mice to UV radiation suppressed the induction of DTH to both erythrocyte and soluble protein antigens injected s.c., but did not suppress the elicitation of the response. The suppressive effect was abrogated by cyclophosphamide treatment. In addition, antigen-specific suppressor cells were found in the spleens of the mice with a decreased DTH response. Since the ability to mount a DTH response has been linked with the resistance to certain pathogenic microorganisms, we suggest that the suppression of DTH by UV radiation may have the potential to compromise host resistance to such infectious agents. 相似文献