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.

Digestibility, nutrient balance and urinary purine derivative excretion in dry yak cows fed oat hay at different levels of intake

A feeding trial A as conducted at the farm of Qinghai Academy of Animal and Veterinary Science, Xining, China during 1996 - 1997 with three dry yak cows (initial body weight 163 - 197 kg, age 5 - 6 years) by using 3 x 3 Latin Square Design to determine the effect of levels of feed intake on digestion, nitrogen balance and purine derivative excretion in urine of yak cows. The animals were fed oat hay (nitrogen 13.5 g/kg dry matter (DM), metabolisable energy 8.3 MJ/kg DM), i.e., 0.3, 0.6 and 0.9 of voluntary intake (VI). Each intake treatment lasted for 17 days and the samples (feeds, faeces and urine) were collected during last 7 days of each period. The results indicate that digestibility of dietary DM, OM, NDF and ash declined when intake levels increased from 0.3 to 0.9 VI [DM, from 66.1% to 59.1% (P < 0.05); OM, from 68.1% to 59.9% (P < 0.05); NDF, from 62.1% to 54.3% (P < 0.05); and ash, from 33.9% to 11.8% (P < 0.05)]. Around 0.10 g N/kg W-0.75 was deficient daily in yak cows at 0.3 VI, and positive N balances were observed at 0.6 and 0.9 VI. Intake levels significantly (P < 0.05) affected total PD excretion in yak urine. The proportion of allantoin increased (P < 0.05) and uric acid decreased (P < 0.05) as intake level of feed increased. (C) 2004 Elsevier B.V. All rights reserved.

Gas chromatographic enantiomer separation on single and mixed cyclodextrin derivative chiral stationary phases

Capillary gas chromatographic enantiomer separation of some polar compounds, including alpha-phenylethylamine, styrene oxide, pyrethroid insecticides and other carboxylates, was investigated on modified cyclodextrin (CD) chiral stationary phases. The chiral stationary phases studied included permethylated beta-CD (PMBCD), heptakis (2,6-di-O-butyl-3-O-butyryl)-beta-CD (DBBBCD), heptakis (2,6-di-O-nonyl-3-O-trifluoroacetyl)-beta-CD (DNTBCD), the mixture of PMBCD and DBBBCD, and the mixture of PMBCD and DNTBCD. On the mixed chiral stationary phases containing the mixtures of derivatized cyclodextrins, enantiomer separation was improved significantly for some compounds as compared to the single cyclodextrin derivative chiral stationary phases, and synergistic effects were observed for some compounds on the mixed cyclodextrin derivative chiral stationary phases.

NMR studies on synthesized diosgenyl saponin analogs

The identification of six synthesized diosgenyl saponin analogs with up to five sugars was accomplished by NMR studies. A combination of homo- and heteronuclear two-dimensional NMR techniques was utilized to achieve the complete H-1 and C-13 NMR assignments. Copyright (C) 2000 John Wiley & Sons, Ltd.

Low temperature X-ray structures of two crystalline forms (I) and (II) of the pyrimidine derivative and sodium channel blocker BW1003C87: 5-(2,3,5-trichlorophenyl)-2,4-diaminopyrimidine

The X-ray crystal structures of two crystalline forms of 5-(2,3,5-trichlorophenyl)-2,4-diaminopyrimidine, C10H7Cl3N4 (code name BW1003C87) (I) and (II), have been carried out at liquid nitrogen temperature. A detailed comparison of the two structures is given. Both are centrosymmetric, with structure (I) in the triclinic space group P (1) over bar unit cell a = 6.4870(10), b = 9.216(2), c = 12.016(2) angstrom, alpha = 75.78(3)degrees, beta = 89.95(3)degrees, gamma = 83.45(3)degrees, V = 691.5(2) angstrom(3), Z = 2 and density (calculated) = 1.544 Mg/m(3); and (II) in the monoclinic space group P2(1)/c, unit cell a = 12.000(2), b = 7.518(2), c = 13.450(3) angstrom, beta = 97.87(3)degrees, V = 1202.0(5) angstrom(3), Z = 4, Density (calculated) = 1.600 Mg/m(3). Structure (I) includes a solvated CH3OH in the lattice. Final R indices [I > 2sigma(I)] are R1 = 0.0427, wR2 = 0.1075 for (I) and R1 = 0.0487, wR2 = 0.1222 for (II). R indices (all data) are R1 = 0.0470, wR2 = 0.1118 for (I) and R1 = 0.0623, wR2 = 0.1299 for (II). 5-Phenyl-2,4 diaminopyrimidine and 6-phenyl-1,2,4 triazine derivatives, which include lamotrigine (3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazine), have been investigated for some time for their effects on the central nervous system. Both lamotrigine and 5-(2,3,5-trichlorophenyl)-2,4-diaminopyrimidine (code name BW1003C87), the subject of the present study, are anticonvulsant as well as neuroprotective in models of brain ischaemia and in a model of white matter ischaemia. BW1003C87 is a sodium channel blocker which also reduces the release of the neurotransmitter glutamate. The three dimensional structures reported here form part of a newly developed data base for the detailed investigation of members of this drug family and their biological activities.

A novel application of ratio spectra derivative spectroscopy for the determination of amphotericin in highly icteric plasma.

Derivative spectroscopy has been utilised for the determination of amphotericin in various biological matrices including plasma, serum, urine and brain tissue. Whilst these methods have all been shown to be suitable for the determination of the drug in these matrices it has been reported that the application fails in the case of highly icteric plasma, this being due to the presence of high concentrations (>50 mu M) of bilirubin. This paper details the application of ratio spectra derivative spectroscopy to overcome the interference of bilirubin with amphotericin in such situations.