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41.
S B Roy Shailendra Kumar A K Pradhan P Chaddah Ram Prasad N C Soni Kalyan Adhikary 《Pramana》1993,41(1):51-60
We present measurements of harmonic generation in the magnetization of sintered pellets of YBa2Cu3O7 and Bi1.7Pb0.3Sr2Ca2Cu3O10 as a function of DC field. The DC field is applied in the field-cooled mode. Measurements are made at 77 K for various values
of the AC field amplitude. A comparison is made with calculations done within the critical state model. 相似文献
42.
Chandan Adhikary Rajesh Bera Buddhadeb Dutta Sreyashi Jana Gabriele Bocelli Andrea Cantoni Siddhartha Chaudhuri Subratanath Koner 《Polyhedron》2008
Three copper(II) Schiff-base complexes, [Cu(L1)(H2O)](ClO4) (1), [Cu(L2)] (2) and [Cu(L3)] (3) have been synthesized and characterized [where HL1 = 1-(N-ortho-hydroxy-acetophenimine)-2-methyl-pyridine], H2L2 = N,N′-(2-hydroxy-propane-1,3-diyl)-bis-salicylideneimine and H2L3 = N,N′-(2,2-dimethyl-propane-1,3-diyl)-bis-salicylideneimine]. The structure of complex 1 has been determined by single crystal X-ray diffraction analysis. In complex 1, the copper(II) ion is coordinated to one oxygen atom and two nitrogen atoms of the tridentate Schiff-base ligand, HL1. The fourth coordination site of the central metal ion is occupied by the oxygen atom from a water molecule. All the complexes exhibit high catalytic activity in the oxidation reactions of a variety of olefins with tert-butyl-hydroperoxide in acetonitrile. The catalytic efficacy of the copper(II) complexes towards olefin oxidation reactions has been studied in different solvent media. 相似文献
43.
Visible light driven amide synthesis in water at room temperature from Thioacid and amine using CdS nanoparticles as heterogeneous Photocatalyst
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Sudipto Das Shounak Ray Abhisek Brata Ghosh Partha Kumar Samanta Suvendu Samanta Bibhutosh Adhikary Papu Biswas 《应用有机金属化学》2018,32(3)
Highly efficient photocatalytic thioacid mediated amide synthesis at room temperature using CdS nanoparticles as photocatalyst was observed under a household 30 W CFL in water. The operationally mild reaction was tolerant to a number of functional group substitutions on amine and could be scaled up to gram. This heterogeneous photocatalyst was extremely stable and could easily be recovered by simple centrifugation for at least six recycling reactions without any significant loss of catalytic performance. The possible reaction mechanism for the photocatalytic thioacid mediated amide synthesis over the CdS semiconductor has also been proposed on the basis of experimental observations. 相似文献
44.
45.
Raju Mukherjee Laxmi Adhikary Anand Khedkar Harish Iyer 《Rapid communications in mass spectrometry : RCM》2010,24(7):879-884
Aspartic acid formed by nonenzymatic deamidation of asparagine often isomerizes to isoaspartic acid through a succinimide intermediate. Accumulation of isoaspartic acid initiates aggregation and degradation in proteins. Deamidation at the antigen‐binding region reduces the efficacy and also upregulates immunogenicity of monoclonal antibodies. We report an improved ‘bottom‐up’ tandem mass spectrometric method to detect and decipher the position of isoaspartate formation in therapeutic immunoglobulin gamma in a single chromatographic run. Differentiation between aspartate and isoaspartate residues through collision‐induced tandem mass spectrometry is formidable due to their identical mass. Signature backbone cleavage ions, cn + 57 and zl–n ? 57, produced upon radical‐mediated fragmentation, were used to delineate the site of isomerization. It is more conclusive than monitoring the relative peak intensity and the decrease in hydrophobicity of the isoaspartate‐containing peptide in a chromatographic elution. Collectively, this methodology provides a useful tool to monitor deamidation and isomerization in biopharmaceuticals during their production, downstream processing and storage. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
46.
The reaction of 9,10-phenanthrenequinone (PQ) with [M(II)(H)(CO)(X)(PPh(3))(3)] in boiling toluene leads to the homolytic cleavage of the M(II)-H bond, affording the paramagnetic trans-[M(PQ)(PPh(3))(2)(CO)X] (M = Ru, X = Cl, 1; M = Os, X = Br, 3) and cis-[M(PQ)(PPh(3))(2)(CO)X] (M = Ru, X = Cl, 2; M = Os, X = Br, 4) complexes. Single-crystal X-ray structure determinations of 1, 2·toluene, and 4·CH(2)Cl(2), EPR spectra, and density functional theory (DFT) calculations have substantiated that 1-4 are 9,10-phenanthrenesemiquinone radical (PQ(?-)) complexes of ruthenium(II) and osmium(II) and are defined as trans-[Ru(II)(PQ(?-))(PPh(3))(2)(CO)Cl] (1), cis-[Ru(II)(PQ(?-))(PPh(3))(2)(CO)Cl] (2), trans-[Os(II)(PQ(?-))(PPh(3))(2)(CO) Br] (3), and cis-[Os(II)(PQ(?-))(PPh(3))(2)(CO)Br] (4). Two comparatively longer C-O [average lengths: 1, 1.291(3) ?; 2·toluene, 1.281(5) ?; 4·CH(2)Cl(2), 1.300(8) ?] and shorter C-C lengths [1, 1.418(5) ?; 2·toluene, 1.439(6) ?; 4·CH(2)Cl(2), 1.434(9) ?] of the OO chelates are consistent with the presence of a reduced PQ(?-) ligand in 1-4. A minor contribution of the alternate resonance form, trans- or cis-[M(I)(PQ)(PPh(3))(2)(CO)X], of 1-4 has been predicted by the anisotropic X- and Q-band electron paramagnetic resonance spectra of the frozen glasses of the complexes at 25 K and unrestricted DFT calculations on 1, trans-[Ru(PQ)(PMe(3))(2)(CO)Cl] (5), cis-[Ru(PQ)(PMe(3))(2)(CO)Cl] (6), and cis-[Os(PQ)(PMe(3))(2)(CO)Br] (7). However, no thermodynamic equilibria between [M(II)(PQ(?-))(PPh(3))(2)(CO)X] and [M(I)(PQ)(PPh(3))(2)(CO)X] tautomers have been detected. 1-4 undergo one-electron oxidation at -0.06, -0.05, 0.03, and -0.03 V versus a ferrocenium/ferrocene, Fc(+)/Fc, couple because of the formation of PQ complexes as trans-[Ru(II)(PQ)(PPh(3))(2)(CO)Cl](+) (1(+)), cis-[Ru(II)(PQ)(PPh(3))(2)(CO)Cl](+) (2(+)), trans-[Os(II)(PQ)(PPh(3))(2)(CO)Br](+) (3(+)), and cis-[Os(II)(PQ)(PPh(3))(2)(CO)Br](+) (4(+)). The trans isomers 1 and 3 also undergo one-electron reduction at -1.11 and -0.96 V, forming PQ(2-) complexes trans-[Ru(II)(PQ(2-))(PPh(3))(2)(CO)Cl](-) (1(-)) and trans-[Os(II)(PQ(2-))(PPh(3))(2)(CO)Br](-) (3(-)). Oxidation of 1 by I(2) affords diamagnetic 1(+)I(3)(-) in low yields. Bond parameters of 1(+)I(3)(-) [C-O, 1.256(3) and 1.258(3) ?; C-C, 1.482(3) ?] are consistent with ligand oxidation, yielding a coordinated PQ ligand. Origins of UV-vis/near-IR absorption features of 1-4 and the electrogenerated species have been investigated by spectroelectrochemical measurements and time-dependent DFT calculations on 5, 6, 5(+), and 5(-). 相似文献
47.
Supriyo Majumder 《Tetrahedron》2010,66(17):3152-812
A titanium-catalyzed 3-component coupling reaction can be used to generate tautomers of 1,3-diimines. These diimines produced in situ undergo condensation with amidines in a one-pot procedure to provide substituted pyrimidines. Seventeen examples of pyrimidines are provided using this one-pot, 4-component procedure from simple starting materials. In some cases, catalyst architecture can be tuned to control the regioselectivity of the alkyne addition. Finally, the regioselectivity of amidine addition to unsymmetrical 1,3-diimines is discussed. 相似文献
48.
A new azido derivative of a NNO donor tridentate Schiff-base copper(II) complex, [CuL(μ1,1-N3)]n (1) (HL = 1-(N-ortho-hydroxyacetophenimine)-2-(N-ethyl)aminoethane), containing a single end-on μ1,1-azido bridged 1D infinite chain has been synthesized and characterized. X-ray single crystal structure analysis reveals that the complex [CuL(μ1,1-N3)]n (1) is a 1D chain in which neighboring Cu(II) chromophores are related by glide planes and linked by single azido bridges in the EO mode. No measurable magnetic interaction was evidenced in the complex [CuL(μ1,1-N3)]n (1) through variable temperature magnetic susceptibility measurements (10–300 K). The complex was used as an active catalyst for the epoxidation of cyclooctene using tert-butyl-hydroperoxide as an oxidant. The catalytic activity of the complex has been compared in a series of solvents. The results show that in acetonitrile medium, the epoxide was produced in high yield with high selectivity. 相似文献
49.
Adhikary A Kumar A Becker D Sevilla MD 《The journal of physical chemistry. B》2006,110(47):24171-24180
This work reports ESR studies that identify the favored site of deprotonation of the guanine cation radical (G*+) in an aqueous medium at 77 K. Using ESR and UV-visible spectroscopy, one-electron oxidized guanine is investigated in frozen aqueous D2O solutions of 2'-deoxyguanosine (dGuo) at low temperatures at various pHs at which the guanine cation radical, G*+ (pH 3-5), singly deprotonated species, G(-H)* (pH 7-9), and doubly deprotonated species, G(-2H)*- (pH > 11), are found. C-8-deuteration of dGuo to give 8-D-dGuo removes the major proton hyperfine coupling at C-8. This isolates the anisotropic nitrogen couplings for each of the three species and aids our analyses. These anisotropic nitrogen couplings were assigned to specific nitrogen sites by use of 15N-substituted derivatives at N1, N2, and N3 atoms in dGuo. Both ESR and UV-visible spectra are reported for each of the species: G*+, G(-H)*, and G(-2H)*-. The experimental anisotropic ESR hyperfine couplings are compared to those obtained from DFT calculations for the various tautomers of G(-H)*. Using the B3LYP/6-31G(d) method, the geometries and energies of G*+ and its singly deprotonated state in its two tautomeric forms, G(N1-H)* and G(N2-H)*, were investigated. In a nonhydrated state, G(N2-H)* is found to be more stable than G(N1-H)*, but on hydration with seven water molecules G(N1-H)* is found to be more stable than G(N2-H)*. The theoretically calculated hyperfine coupling constants (HFCCs) of G*+, G(N1-H)*, and G(-2H)*- match the experimentally observed HFCCs best on hydration with seven or more waters. For G(-2H)*-, the hyperfine coupling constant (HFCC) at the exocyclic nitrogen atom (N2) is especially sensitive to the number of hydrating water molecules; good agreement with experiment is not obtained until nine or 10 waters of hydration are included. 相似文献
50.
Supriyo Majumder 《Tetrahedron letters》2008,49(11):1771-1772
Cyclooctatetraene is readily synthesized by the oxidation of in situ generated [Li(TMEDA)]2[C8H8] with 1,2-dibromoethane. The product is readily isolated and produced without the use of hazardous or toxic reagents. 相似文献