Synthesis, crystal structure and biological activities of N '-(4-methoxybenzylidene)-2-(1H-1,2,4-triazol-1-yl) acetohydrazide

The title compound, N'-(4-methoxybenzylidene)-2-(1H-1,2,4-triazol-1-yl)acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS,H-1 NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound has a low antifungal activity.

5-[(1H-1,2,4-yriazol-1-yl)methyl]-4-(4-fluorobenzylideneamino)-2H-1,2,4-triazole-3(4H)-thione

In the title compound, C12H10FN7S, the dihedral angles made by the plane of the thione-substituted triazole ring with the planes of the other triazole ring and the benzene ring are 71.94 (3) and 40.10 (2)degrees, respectively. Inter- and intramolecular hydrogen-bond and pi-pi stacking interactions stabilize the structure.

Synthesis and. crystal structure of N '-(4-fluorobenzylidene)-2-(1H-1,2,4-triazole-1-yl) acetohydrazide

N'-(4-fluorobenzylidene)-2-(1H-1 2,4-triazole-1-yl) acetohydrazide was synthesized by the reaction of 4-fluorobenzaldehyde with 2-(1H-1 2,4-triazole-1-yl) acetohydrazide. The structure was confirmed via elemental analysis, MS, H-1 NMR, IR, and X-ray diffraction. It crystallized in a monoclinic system with space group P2 (1) a = 0.4905 (1) nm, b = 0.8160 (2) nm, c = 1.4105 (3) nm, beta = 93.33 (3)degrees, Z = 2, V = 0.5636 (2) nm(3), D-c = 1.457 Mg/m(3), mu = 0.112 mm(-1), F(000) = 256, and final R-1 = 0.0685. Several intermolecular hydrogen-bond interactions existed in the crystal structure, facilitating the stabilization of the compound.

Crystal structure and DFT studies of a triazole derivative: 4-(2-hydrobenzylideneamino)-3-(1,2,4-triazol-4-yl-methyl) 1H-1,2,4-triazole-5 (4H)-thione

A novel triazole derivative 4-(2-hydrobenzylideneamino)-3-(1, 2, 4-triazol-4-ylmethyl)-1H-1, 2, 4-triazole-5 (4H)-thione(1) was synthesized and characterized using elemental analysis, MR, and H-1 NMR, and its crystal structure was determined via X-ray single crystal diffraction analysis. Crystal data: monoclinic, P2 (1)/c, a = 0.83335 (9) nm, b = 1. 49777 (16) run, c = 1. 14724 (12) nm, beta = 107. 990 (2)degrees, D = 1. 470 Mg/m(3), and Z = 4. The geometries and the vibrational frequencies were determined using the density functional theory(DFT) method at the B3LYP/6-31G* level. To demonstrate the accuracy of the reaction route of compound 1, one of the important intermediates was also tested using the same method. The structural parameters of the two compounds calculated using the DFT study are close to those of the crystals, and the harmonic vibrations of the two compounds computed via the DFT method are in good agreement with those in the observed IR spectral data. The thermodynamic properties of the title compound were calculated, and the compound shows a good structural stability at normal temperature. The test results of biological activities show that it has a certain bactericidal ability.

Diisothiocyanatobis(1-vinyl-1H-imidazole-kappa N-3)-copper(II)

In the title compound, [Cu(NCS)(2)(C5H6N2)(2)], each Cu atom is coordinated by two N atoms from two Eim (Eim = 1-vinyl-1H-imidazole) ligands and two N atoms from two isothiocyanate groups. The Cu atom adopts a square-planar geometry. The mean Cu-N(Eim) and Cu-N(NCS) distances are 1.960 (6) and 1.993 (6) angstrom, respectively.

多取代山酮及其糖甙山酮的~1H和~（13）CNMR研究

总结了作者所测定过的多取代酮及其糖甙类衍生物的１Ｈ和13ＣＮＭＲ位移数据．着重就取代基与结构的关系进行了探讨．认为多取代酮１位和８位取代情况直接影响着其他位置的化学位移数值．这一现象可以直接用于该类化合物的结构鉴定．

2-(2-Phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA) and its application for determination of amines by high performance liquid chromatography with fluorescence detection and identification with mass spectroscopy/atmospheric pressure chemical ionization

A simple, sensitive, and mild method for the determination of amino compounds based on a condensation reaction with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC-HCI) as the dehydrant with fluorescence detection has been developed. Amines were derivatized to their acidamides with labeling reagent 2-(2-phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA). Studies on derivatization conditions indicated that the coupling reaction proceeded rapidly and smoothly in the presence of a base catalyst in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maximum at lambda(ex) 260nm and an emission maximum at lambda(em) 380nm. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by high-performance liquid chromatography. Identification of derivatives was carried out by online post-column mass spectrometry (LC/APCI-MS/MS) and showed an intense protonated molecular ion corresponding m/z [MH](+) under APCI in positive-ion mode. At the same time, the fluorescence properties of derivatives in various solvents or at different temperature were investigated. The method, in conjunction with a gradient elution, offered a baseline resolution of the common amine derivatives on a reversed-phase Eclipse XDB-C-8 column. LC separation for the derivatized amines showed good reproducibility with acetonitrile-water as mobile phase. Detection limits calculated from 0.78 pmol injection, at a signal-to-noise ratio of 3, were 3.1-18.2 fmol. The mean intra- and inter-assay precision for all amine levels were < 3.85% and 2.11%, respectively. Excellent linear responses were observed with coefficients of > 0.9996. The established method for the determination of aliphatic amines from real wastewater and biological samples was satisfactory. (c) 2006 Elsevier B.V. All rights reserved.