Synthesis and antibacterial activity of some 5-hydroxy-5-trifluoromethyl-4,5-dihydropyrazol-1-thiocarboxamides, 3-trifluoromethylpyrazol-1-thiocarboxamides and 4-aryl-2-(5(3)-trifluoromethyl-1-pyrazolyl)thiazoles

5-Hydroxy-5-trifluoromethyl-4,5-dihydropyrazol-1-thiocarboxamides 3 and 3-trifluoromethylpyrazol-1-thiocarboxamides 4, regioselectively obtained by the condensation of trifluoromethyl-β-diketones with thiosemicarbazide under neutral and acidic conditions, on further reaction with phenacyl bromides 5 afforded 4-aryl-(5-trifluoromethyl-pyrazol-1-yl)thiazoles 6 and 4-aryl-(3-trifluoromethyl-pyrazol-1-yl)thiazoles 7, respectively. Five 4,5-dihydropyrazoles (3a–e) and two pyrazolylthiazoles (6a and 6c) were tested against one Gram-positive and one Gram-negative bacteria to assess their in vitro antibacterial activity. Compounds 3a, 3b and 3e showed moderate antibacterial activity against Gram-positive bacterium, Bacillus pumilus.     

FeCl3 catalysed two consecutive aminomethylation at the α-position of the β-dicarbonyl compounds: an easy access to hexahydropyrimidines and its spiro analogues

Multicomponent synthesis of 1,3-diaryl-hexahydropyrimidines by a one-pot reaction of 1,3-dicarbonyl compounds, amines and formaldehyde catalysed by FeCl₃ in dichloromethane at room temperature (25-30 °C) has been reported. Double amino methylation occurs at the α-position of the 1,3-dicabonyl compounds/β-keto esters. The same methodology leads to spiro compounds with indane-1,3-dione. In this reaction, six molecules condense in one pot to form six new covalent bonds, thus, creating high atom economy. This is the first report of the synthesis of the substituted hexahydropyrimidines involving β-keto esters and its spiro analogues with indane-1,3-dione.     

An efficient synthesis of pyrazole chalcones under solvent free conditions at room temperature

An easy,safe,solvent free and effective method for the synthesis of pyrazole-substituted chalcones has been achieved by grinding pyrazole aldehydes and acetophenones in the presence of activated barium hydroxide(C-200) in high yield within short span of time.All reactions were carried out just by grinding the two reactants in the presence of activated barium hydroxide(C-200). Results are also compared with sodium hydroxide and potassium hydroxide.     

Comparison of Planar and 3‐D Interdigitated Electrodes as Electrochemical Impedance Biosensors

It has been reported that the introduction of a dielectric barrier between adjacent digits of an interdigitated electrode array can improve the sensitivity of the array as an electrochemical impedance biosensor. Here we present an in‐depth analysis of the impedance in planar interdigitated electrodes and 3‐D interdigitated electrodes (with dielectric barriers). The analysis indicates that the planar geometry not only provides lower impedance but also a higher change impedance as a result of molecular immobilization on the electrode array surface.     

Isolation and biological evaluation of chromone alkaloid dysoline,a new regioisomer of rohitukine from Dysoxylum binectariferum

The chromone alkaloid dysoline (1), a new regioisomer of rohitukine (2) along with rohitukine and rohitukine-N-oxide (3) were isolated from the stem barks of Dysoxylum binectariferum. The structure of dysoline (1) was determined by extensive 2D-NMR studies and the absolute configuration was established by NOESY and CD spectra. Dysoline (1) consisted of a 5,7-dihydroxy-2-methylchromone nucleus substituted with a 2′-hydroxylated N-Me piperidine ring at the C-6 position. Dysoline differs from rohitukine by the position of the piperidine ring on the chromone nucleus. Dysoline displayed promising cytotoxicity in HT1080 fibrosarcoma cells with an IC₅₀ of 0.21 μM, and also displayed significant inhibition of proinflammatory cytokines TNF-α and IL-6.     

Cholesterol biosensor based on amino-undecanethiol self-assembled monolayer using surface plasmon resonance technique

Cholesterol oxidase has been covalently immobilized onto 11-amino-1-undecanethiol hydrochloride (AUT) self-assembled monolayer (SAM) fabricated on gold (Au) substrates using glutaraldehyde as a cross-linker. These ChOx/AUT/Au bioelectrodes characterized using contact angle (CA) measurements; electrochemical technique and atomic force microscopy (AFM) have been utilized for the estimation of cholesterol in solution using the surface plasmon resonance (SPR) technique. These biosensing electrodes exhibiting linearity from 50 to 500 mg/dL of cholesterol in solution and sensitivity of 1.23 m0/(mg dL), can be used more than 20 times and have a shelf life of about 10 weeks when stored at 4 degrees C.     

Blends of POSS-PEO(n=4)(8) and high molecular weight poly(ethylene oxide) as solid polymer electrolytes for lithium batteries

Solid polymer electrolyte blends were prepared with POSS-PEO(n=4)8 (3K), poly(ethylene oxide) (PEO(600K)), and LiClO4 at different salt concentrations (O/Li = 8/1, 12/1, and 16/1). POSS-PEO(n=4)8/LiClO4 is amorphous at all O/Li investigated, whereas PEO(600K) is amorphous only for O/Li = 8/1 and semicrystalline for O/Li = 12/1 and 16/1. The tendency of PEO(600K) to crystallize limited the amount of POSS-PEO(n=4)(8) that could be incorporated into the blends, so that the greatest incorporation of POSS-PEO(n=4)(8) occurred for O/Li = 8/1. Blends of POSS-PEO(n=4)(8)/PEO(600K)/LiClO4 (O/Li = 8/1 and 12/1) microphase separated into two amorphous phases, a low T(g) phase of composition 85% POSS-PEO(n=4)(8)/15% PEO(600K) and a high T(g) phase of composition 29% POSS-PEO(n=4)(8)/71% PEO(600K). For O/Li = 16/1, the blends contained crystalline (pure PEO(600K)), and two amorphous phases, one rich in POSS-PEO(n=4)(8) and one rich in PEO(600K). Microphase, rather than macrophase separation was believed to occur as a result of Li(+)/ether oxygen cross-link sites. The conductivity of the blends depended on their composition. As expected, crystallinity decreased the conductivity of the blends. For the amorphous blends, when the low T(g) (80/20) phase was the continuous phase, the conductivity was intermediate between that of pure PEO(600K) and POSS-PEO(n=4)(8). When the high T(g) (70/30, 50/50, 30/70, and 20/80) phase was the continuous phase, the conductivity of the blend and PEO(600K) were identical, and lower than that for the POSS-PEO(n=4)(8) over the whole temperature range (10-90 degrees C). This suggests that the motions of the POSS-PEO(n=4)(8) were slowed down by the dynamics of the long chain PEO(600K) and that the minor, low Tg phase was not interconnected and thus did not contribute to enhanced conductivity. At temperatures above T(m) of PEO(600K), addition of the POSS-PEO(n=4)(8) did not result in conductivity improvement. The highest RT conductivity, 8 x 10(-6) S/cm, was obtained for a 60% POSS-PEO(n=4)(8)/40% PEO(600K)/LiClO4 (O/Li = 12/1) blend.     

Synthesis, spectral and oxidase studies of a new diamide copper(II) complex with pendant benzimidazolyl groups

A new benzimidazole-based diamide ligand-N,N'-bis(alanine-2-benzimidazolyl) hexanediamide (ABHA) has been synthesized and utilized to prepare Cu(II) complexes of general composition [Cu(ABHA)X2].nH2O,where X is an exogenous anionic ligand (X=Cl-,NO3-). Low temperature EPR spectra has been obtained that shows gparallel>gperpendicular>2.0024, indicating a tetragonal geometry in the solution state. The complexes display a quasi-reversible redox wave due to the Cu(II)/Cu(I) reduction process. E1/2 values shift anodically as NO3-相似文献   

Unexpected ambidoselectivity in crossed-aldol reactions of α-oxy aldehyde trichlorosilyl enolates

The ambido-, stereo- and enantioselectivity of the phosphoramide-promoted aldol reactions of α-oxy aldehyde trichlorosilyl enolates with benzaldehyde has been investigated. Analysis of the products from α-tert-butyldimethylsilyloxy α-deuterioacetaldehyde trichlorosilyl enolate confirmed that this 1,2-bis-silyloxyethene derivative reacted as a tert-butyldimethylsilyl enolate rather than trichlorosilyl enolate in the aldol reaction with very high ambidoselectivity. The phosphoramide-coordinated trichlorosilyl group acted as an organizing center for the aldol reaction. From the aldol process, excellent anti-diastereoselectivity could be achieved. The enantioselectivity remained moderate to low for both anti- and syn-diastereomer with a wide range of phosphoramide catalysts. α-Triisopropylsilyloxy, phenoxy and benzyloxy acetaldehyde trichlorosilyl enolates also reacted in a similar fashion with benzaldehyde to give aldol products with varying degrees of selectivities.