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Pd/C/PPh3: A Simple and Efficient Catalyst System for Double Carbonylation Reactions
- Pages: 623-627
- First Published: 06 May 2009

The double carbonylation of iodobenzene and diethylamine proceeds smoothly in the presence of Pd/C and carbon monoxide to afford the corresponding α-keto amide in good yields with excellent selectivity. In addition, other aryl iodides and secondary amines also react under similar conditions to form α-keto amides in good yields.
Evaluation and Comparison of a 3,5-Dimethylphenyl Isocyanate Teicoplanin and Phenyl Isocyanate Teicoplanin Chiral Stationary Phases
- Pages: 628-632
- First Published: 06 May 2009

Two chiral stationary phases (CSP), phenylisocyanate teicoplanin CSP (Ph-TE), and 3,5-dimethylphenyl isocyanate teicoplanin CSP (DMP-TE) were prepared from the macrocyclic glycopeptide teicoplanin CSP (TE) using derivative agents, phenyl isocyanate or 3,5-dimethylphenyl isocyanate, respectively. The evaluation and comparison of these two self-made CSP were performed using HPLC enantiomeric separations in two different mobile phase modes. Twelve racemic analytes, including eight amino acids and four non-amino acid compounds reached enantioseparation using the RPLC mobile phase and six amino alcohols reached enantiomeric separation using the PO mobile phase. Because of similar structure, the Ph-TE and DMP-TE have similar chiral separation ability.
Reactivity of Carboxyl-functionalized Cubane-like Photocyclodimer of 2-Substituted Naphthalene toward Aromatic Amines
- Pages: 633-637
- First Published: 06 May 2009

Carboxyl-functionalized cubane-like photocyclodimer 2 was reacted with a series of aromatic amines 3 for understanding the reactivity of this unique system. Spectroscopic and X-ray crystal structural analyses demonstrate that N,N′-dicyclohexylcarbodiimide (DCC) is reactive toward 2 affording stable 4 with a well-retained cubane-like structure. With the assistance of DCC, mono- and diacyl-substituted photocyclodimers of 2-naphthalene (5 and 6) have also been achieved in reasonable yields in addition to the formation of 4. Subtle change in electronic properties of the series of aromatic amines 3 modulates the reactivity and product distribution remarkably.
Full Papers
Kinetic Study of the Electro-Catalytic Oxidation of Hydrazine on Cobalt Hydroxide Modified Glassy Carbon Electrode
- Pages: 638-644
- First Published: 06 May 2009

The pseudo-steady state polarization curves of the electro-oxidation of hydrazine CHM-GC electrode at a number of hydrazine concentrations are presented in the left figure. The oxidation process was found to begin at nearly 470 mV (vs. SCE) and to reach a plateau at 605 mV (vs. SCE), while the oxygen evolution starts at still higher potentials. In the course of reaction the coverage of Co(IV) increases and reaches a saturation (steady state) level and the oxidation current follows accordingly.
Thixotropic and Viscoelastic Properties of Hydrotalcite Like Compound-Montmorillonite Suspensions
- Pages: 645-648
- First Published: 06 May 2009

The thixotropic and viscoelastic properties of the complex suspension made up of hydrotalcite-like compound (HTlc)- sodium montmorillonite (MT) suspensions have been studied carefully. Two kinds of Fe-Mg-Al-HTlc systems have been examined, and from sample 1 to sample 2, the content of Mg2+ enhances gradually while the ratio of Al to Fe remains constant. With increasing the content of Mg2+ in the HTlc samples, the results of the creep tests and the stress sweep experiments all indicate that the structure strength of the HTlc/MT suspension rises. Moreover, the hysterisis loops have been detected carefully, showing that the thixotropic degree increases with increasing the Mg2+ content. It was concluded that the rheological properties could be adjusted by the change of the metal content.
Dynamical Complexity in Electrochemical Oxidations of Thiocyanate
- Pages: 649-654
- First Published: 06 May 2009
Electrochemical Impedance Spectroscopic Measurements of Sexithiophene–Effect of the Electrode Nature and the Dopant (CuCl2) Content
- Pages: 655-659
- First Published: 06 May 2009

Electrochemical impedance spectroscopic (EIS) measurements of sexithiophene (6T) were carried out according to the Pt/6T/M sandwich structure configuration, for various electrode materials (M=GC, ITO, Ag, Cu, Al) and for different doping levels of copper chloride (CuCl2). The results demonstrate that two types of charge transport are involved in the redox process at the electrode/6T interface and inside the bulk oligomer. The complex-plane impedance plots obtained for various doping levels of CuCl2 exhibit arc shapes. The charge-transfer resistance measured from the diagrams decreases systematically with the addition of the salt, leading to an increase of the oligothiophene conductivity.
A Theoretical Investigation on the Reaction Mechanism of the C9H12+· Side-chain Decomposition
- Pages: 660-664
- First Published: 06 May 2009

n-Phenylpropane cation C9H12+· serves as a prototype to investigate the reaction mechanisms of alkylbenzene cations. The decomposition reactions of C9H12+· system have been studied extensively at the B3LYP/6-311++G∗︁∗︁ level with Gaussian 98 program package. The reaction mechanism show C9H12+·→C7H7+ +C2H5·, which is thermodynamically most favorable.
Non-isothermal Decomposition Kinetics, Specific Heat Capacity and Adiabatic Time-to-explosion of 1-Amino-1-hydrazino-2,2-dinitroethylene (AHDNE)
- Pages: 665-671
- First Published: 06 May 2009

1-Amino-1-hydrazino-2,2-dinitroethylene (AHDNE) has no melting point, and its thermal behavior can be divided into two conterminous intensely exothermic decomposition stages. The peak temperatures are 112.95 and 133.73 °C at the heating rate of 5.0 °C·min−1, respectively. The whole enthalpy of exothermic decomposition reaction of AHDNE is about 1785.4 J·g−1, and the non-isothermal kinetic equation of the first exothermic decomposition reaction of AHDNE is dα/dT=1019.29(1−α)exp(−1.88×104/T)/β.
Calorimetric Study and Thermal Analysis of 4-(Aminomethyl) Benzoic Acid
- Pages: 672-676
- First Published: 06 May 2009

The molar heat capacities of 4-(aminomethyl)benzoic acid were measured over the temperature range from 80 to 400 K by adibadic calorimetry. The heat capacity curve was smooth and no any thermal anomaly was observed, which means that the compound is stable in this temperature range. Heat capacity data (J·K−1·mol−1) were fitted to a polynomial equation: Cp,m=162.01+91.771X+6.4372X2+1.7517X3−4.991X4+8.909X5+1.585X6, X= (T−235)/155. The ststandard enthalpy of formation of the compound was determined to be −(420±5) kJ·mol−1, through combustion calorimetry.
Sm1.5Sr0.5MO4 (M=Ni, Co, Fe) Cathode Catalysts for Ammonia Synthesis at Atmospheric Pressure and Low Temperature
- Pages: 677-680
- First Published: 06 May 2009

Sm1.5Sr0.5MO4 (M=Ni, Co, Fe) (SSM) was prepared by a sol-gel method and characterized by XRD measurements. Ammonia was synthesized from wet hydrogen and desiccated nitrogen by electrochemistry at atmospheric pressure and low temperature. The Sm1.5Sr0.5NiO4 (SSN) was the better cathode catalyst than Sm1.5Sr0.5CoO4 (SSC) and Sm1.5Sr0.5FeO4 (SSF) in ammonia synthesis by electrochemistry.
Spectroscopic Studies on the Binding of Bacteriophage Mequindox with Bovine Serum Albumin
- Pages: 681-686
- First Published: 06 May 2009
A Theoretical Study on the Vibrational Spectra and Thermodynamic Properties for the Derivatives of HNS
- Pages: 687-696
- First Published: 06 May 2009

At the DFT-B3LYP/6-31G∗︁ level, the IR spectra of the derivatives of HNS were obtained and assigned by vibrational analysis. The calculated and experimental infrared spectra of HNS were compared, and it is found that they were all close, which proves the reliability of theoretical computation. On the basis of the conlusion, the thermodynamic properties were evaluated.
π Type Lithium Bond Interaction between Ethylene, Acetylene, or Benzene and Amido-lithium
- Pages: 697-702
- First Published: 06 May 2009
Adsorption of Methane on Water under Hydrate Formation Conditions
- Pages: 703-706
- First Published: 06 May 2009

The interfacial properties between methane and water were investigated systemically under hydrate formation conditions. Pressure has a great influence upon the interface tension at higher pressure. Higher pressure and lower temperature corresponded to higher adsorption concentration of methane. The adsorption of methane on water under hydrate formation condition is more preferable than that at 298.2 K.
Activity Coefficients for NaBr in Aqueous D-Trehalose/D-Cellobiose Solutions at 298.15 K
- Pages: 707-712
- First Published: 06 May 2009

The ionic mean activity coefficients of NaBr in trehalose-water and cellobiose-water mixtures have been experiment- ally determined at 298.15 K from electrochemical potential measure- ments by an electrochemical cell containing two ion selective electrodes (ISE), together with the activity coefficients of the disaccharides. The parameters C1 representing the pair interactions between the disaccharides and NaBr have been obtained. The interactions of NaBr with trehalose, cellobiose and glucose were compared and discussed in terms of their difference in the stereo-structures.
Molal Enthalpy of Solution of Ionic Liquid [C2mim][GaCl4]
- Pages: 713-716
- First Published: 06 May 2009
Preparation and Storage of Silver Nanoparticles in Aqueons Polymers
- Pages: 717-721
- First Published: 06 May 2009
Silver(I) Coordination Polymers of 2,11-Dithia[3.3]paracyclophane and in situ Silver(I) Perfluoro-dicarboxylates
- Pages: 722-726
- First Published: 06 May 2009
![Silver(I) Coordination Polymers of 2,11-Dithia[3.3]paracyclophane and in situ Silver(I) Perfluoro-dicarboxylates](/cms/asset/40aa8cdb-0602-4867-87dc-215a8bc64814/mcontent.jpg)
Coordination polymers of 2,11-dithia[3.3]- paracyclopane (dtpcp) with in situ silver(I) perfluoro-dicarboxylates characterized by single crystal X-ray analysis are described. With disilver(I) tetrafluorosuccinate [(CF2)n- (COOAg)2, n=2], 1D chains of [Ag4(dtpcp)3- (C2F4(CO2)2)2]·2CH3OH (1) are given. Changing the silver salt to disilver(I) hexafluoroglutarate [(CF2)n(COOAg)2, n=3] produces a 3D structure with composition of [Ag2(dtpcp)(C3F6(CO2)2)] (2). With disilver(I) octafluoroadipate [(CF2)n(COOAg)2, n=4], 2D porous sheets with cavities, in which guest mesitylene molecules are located, are formed.
Effect of Pb2+ on the Kinetic and Spectral Characterization of Ribulose-1,5-bisphosphate Carboxylase/Oxygenase
- Pages: 727-731
- First Published: 06 May 2009
Monitoring of Methyldopa by Fast Fourier Transform Continuous Cyclic Voltammetry at Gold Microelectrode
- Pages: 732-738
- First Published: 06 May 2009
Controlled Synthesis and Characterization of Monodisperse Fe3O4 Nanoparticles
- Pages: 739-744
- First Published: 06 May 2009
Determination of Epinephrine by Flow Injection Analysis Coupled Ag(III) Complex-Luminol Chemiluminescence Detection
- Pages: 745-750
- First Published: 06 May 2009

It was discovered that chemiluminescence greatly increased when the epinephrine solution was injected into a mixture of [Ag(HIO6)2]5− and alkaline luminol. Based on this finding, a simple, sensitive and rapid flow-injection analysis CL assay for epinephrine was developed. The limit of detection of this method was 8.0×10−10 mol·L−1 for epinephrine and the RSD was 2.9% for 1.5×10−8 mol·L−1 epinephrine. Based on the free radical trapping experiment, the mechanism of the reactions was also discussed.
NMR-based Metabonomic Study on Rat's Urinary Metabolic Response to Dosage of Triptolide
- Pages: 751-758
- First Published: 06 May 2009

NMR-based metabonomic approach was used to examine rat's urinary response to dosage of triptolide, a major component responsible for the immunosuppressive and anti- inflammatory effects of Tripterygium wilfordii Hook F. The results are shown by PCA score plot. It was obvious that biochemical variation induced by TP was time-related, and the maximal alteration in metabolite appeared at 16 h later after dosage, and partially recovered 56 h later after dosage.
Separation of Aminobenzoic Acids by Gold Nanoparticle- modified Capillary Electrophoresis
- Pages: 759-762
- First Published: 06 May 2009

A novel separation method for aminobenzoic acids by capillary electrophoresis was developed. The capillary was modified with gold nanoparticles. The effect of gold nanoparticles on the resolution and selectivity of separation was investigated. The presence of gold nanoparticle improved the precision of the analysis and increased the separation efficiency. Under the optimized experiment conditions, aminobenzoic acids were separated and determined in a running buffer containing 5 mmol·L−1 sodium dihydrogen phosphate and 0.236 µmmol·L−1 gold nanoparticles at pH 5.3.
A Simple Design to Realize Micro-column Separation by Conventional Analytical HPLC
- Pages: 763-767
- First Published: 06 May 2009

Porous inlet frit in a fused silica capillary could be prepared by sintering stainless steel powders under 500 meshes for about 20 s. The use of such frits or metal meshes in capillary to retain C18 particles was demonstrated to be stable and specially robust with continuous packing over 60 MPa and long chromatographic runs.
Removal of Chloroform from Hydrochloride Acid Solution Using Fine Powder of Polymer as Adsorbent
- Pages: 768-772
- First Published: 06 May 2009

The adsorptive ability of some fine powder of polymer adsorbents, viz. polyvinylchloride (PVC), chlorinated rubber (CR), porous polypropylene (PP), chlorinated polypropylene (CPP), and solid paraffin (SP), for chloroform was investigated in terms of their adsorption isotherms in 20% hydrochloric acid solutions at 298.15 K. The adsorptivity of PVC and CR was nearly equivalent to that of active carbon with their saturated adsorption being about 1.4 g-CHCl3 (g-absorbent)−1, indicating that the commercial polymer powder of PVC or CR can be used as an efficient absorbent for the removal of chloroform from its aqueous solution.
Determination of Bioactive Components in Polygonum perfoliatum L. by Capillary Electrophoresis with Electrochemical Detection
- Pages: 773-776
- First Published: 06 May 2009

Five bioactive components (ferulic acid, vanillic acid, quercetin, caffeic acid and protocatechuic acid) in Polygonum perfoliatum L. were simultaneously determined by capillary electrophoresis with electrochemical detection. Effects of several important factors such as pH and concentration of running buffer, separation voltage, injection time and detection potential were investigated to acquire the optimum conditions. This proposed method could be successfully used for the determination of the analytes in Polygonum perfoliatum L. with satisfactory results.
Separation of Immunoglobulin in Conjunction with High Performance Liquid Chromatography Using Poly(vinyl ester resin) Monolith
- Pages: 777-780
- First Published: 06 May 2009

Using vinyl ester resin both as the monomer and the cross-linker, 2,2-azobis(2- methylprnopionitrile) (AIBN) as initiator, poly(vinyl ester resin) monolithic column was prepared to separate the IgG and IgY from human plasma and egg yolk by HPLC respectively. The influence of concentration and pH of mobile phase on the chromatographic performance was investigated. The results suggested that such kind of monolithic column could be used as a simple, cheap, effective method for the separation and purification of IgG. It is a good kind of stationary phase for HPLC.
Development and Validation of Selective Spectrophotometric Methods for the Determination of Pregabalin in Pharmaceutical Preparation
- Pages: 781-786
- First Published: 06 May 2009
Three simple, quick and sensitive methods are described for the spectrophotometric determination of pregabalin (Pgb) in pharmaceutical preparations. Among them, the first two methods are based on the reaction of Pgb as n-electron donors with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and 7,7,8,8-tetracyanoquinodi- methane (TCNQ) as π-acceptors to give highly colored complex species. The colored products were quantitated spectrophotometrically at 494 and 841 nm for DDQ and TCNQ, respectively. Beer's law was obeyed in the concentration ranges 2.0–30.0 and 1.5–10 g·mL−1 for DDQ and TCNQ methods, respectively. The third method is based on the interaction of ninhydrin (NN) with primary amine present in the pregabaline. This reaction produces a blue coloured product in N,N-dimethylformamide (DMF) medium, which absorbs maximally at 573 nm. Beer's law was found in the concentration range 40.0–180.0 µg·mL−1. The methods were applied successfully to the determination of this drug in pharmaceutical dosage forms.
Facile Synthesis of 1,2,3,4-Tetrahydrobenzo[b][1,8]-naphthyridin-2-one via Baylis-Hillman Adducts
- Pages: 787-790
- First Published: 06 May 2009
![Facile Synthesis of 1,2,3,4-Tetrahydrobenzo[b][1,8]-naphthyridin-2-one via Baylis-Hillman Adducts](/cms/asset/bee4c417-5c11-4a35-a56b-4ab8a86681d2/mcontent.jpg)
Various benzo[b][1,8]naphthyridin-2-ones were synthesized by a one-pot tandem reduction-double cyclization from the corresponding (Z)-ethyl 4-cyano-5-(2-nitrophenyl)- pent-4-enoates, which were easily prepared via Johnson-Claisen rearrangement from Baylis-Hillman affixtures of 2-nitrobenzaldehydes. The procedure has the advantages of easy handling and seperation under mild and green conditions, and the overall yields are moderate.
Synthesis of β-Hydroxy Sulfides via Thiolysis of Epoxides Using S-Alkylisothiouronium Salts as Thiol Equivalents in Basic Aqueous Medium
- Pages: 791-796
- First Published: 06 May 2009
Fragmentation Study of 2-Amino-4H-1,3-oxazines and Octahydro-4-phenyl-2H-pyrano[2,3-d]pyrimidin-2-ones: Identification of Heterocyclic Six-membered Ring in Three-component Reactions
- Pages: 797-804
- First Published: 06 May 2009
Site-directed PEGylations of Thymosin α 1 Analogs and Evaluation of Their Immunoactivity
- Pages: 805-809
- First Published: 06 May 2009
Synthesis and Bioactivity of Some New 2-(Alkoxy carbonyl alkyl)-6-bromo-3,4-dihydro-3-(α-methyl benzyl)-2-oxo-benzo[e] [2H-1,3,2-oxazaphosphinine] Derivatives
- Pages: 810-814
- First Published: 06 May 2009
Synthesis of some new 2-(alkoxy carbonyl alkyl)-6-bromo-3,4-dihydro-3-(α-methyl benzyl)-2-oxo-3-benzo[e][2H-1,3,2-oxazaphosphinine] derivatives was accomplished through a two step process, which involves the condensation of 2-[(α-methylbenzyl amino)methyl]-4-bromophenol (1) with phosphorus oxychloride in equimolar quantities in the presence of triethylamine in dry toluene in 50–55 °C producing the corresponding intermediate (2), and subsequent reaction with the amino acid alkyl ester in dry tetrahydrofuran in the presence of triethylamine at different temperatures. They exhibited significant antibacterial and fungal activity.
Preparation and Application of Perchloric Acid Supported on Alumina (Al2O3-HClO4) to the Synthesis of α-(α-Amidobenzyl)-β-naphthols
- Pages: 815-820
- First Published: 06 May 2009

Preparation of perchloric acid supported on alumina and its primary application as a solid supported heterogeneous catalyst to the synthesis of α-(α-amidobenzyl)-β-naphthols by a one-pot, three-component condensation of benzaldehydes, β-naphthol and acetamide or benzamide under thermal solvent-free conditions were described. The present methodology offers several advantages such as simple procedure, shorter reaction time, and excellent yields.
PPA-SiO2 Catalyzed Multi-component Synthesis of N-[α-(β-Hydroxy-α-naphthyl)(benzyl)] O-Alkyl Carbamate Derivatives
- Pages: 821-824
- First Published: 06 May 2009
![PPA-SiO2 Catalyzed Multi-component Synthesis of N-[α-(β-Hydroxy-α-naphthyl)(benzyl)] O-Alkyl Carbamate Derivatives](/cms/asset/8e84cb99-f23b-4615-9cae-afd2ed23b707/mcontent.jpg)
Silica-supported polyphosphoric acid (PPA-SiO2) was found to be an efficient catalyst for the multi-component condensation reaction of benzaldehydes, 2-naphthol, and methyl/benzyl carbamate and to afford the corresponding N-[α-(β-hydroxy-α- naphthyl)(benzyl)] O-alkyl carbamate derivatives in good to excellent yields. This new approach consistently has the advantage of short reaction time, high conversions, clean reaction profiles, and simple experimental and work-up procedures.
Design and Synthesis of Matrix Metalloprotease Photoaffinity Trimodular Probes
- Pages: 825-833
- First Published: 06 May 2009

The rational designed trimodular probe 2 with three functional groups for target recognition, proximal target cross-linking and distal reporter tag attachment via click chemistry of a photo-stable azido-acetyl group demonstrates specificity, sensitivity, and the potential of general application in activity-based protein profiling for Matrix Metalloprotease.
An Efficient Four-Component, One-Pot Synthesis of Poly-Substituted Pyrimidines in Water
- Pages: 834-838
- First Published: 06 May 2009
Experimental Study on the Molecular Dimension and Configuration of Polymer and Its Flow Characteristics from Electrolyte Effect
- Pages: 839-845
- First Published: 06 May 2009

As shown in the scheme, this paper mainly studied the molecular dimension and configuration of polymer from electrolyte effect, and took a further study on the polymer viscosity and flow characteristics of polymer solution in the porous medium, which will provide a guideline for designing the polymer flooding performance in oilfields.
Notes
Synthesis and Properties of Heteroacenes Containing Pyrrole and Thiazine Rings as Promising n-Type Organic Semiconductor Candidates
- Pages: 846-849
- First Published: 06 May 2009

Two trifluoromethyl substituted PBBTZ derivatives 3a and 3b were facilely synthesized and characterized. Their optical, electrochemical and thermal properties were studied. The low energy levels render them well air-stable, and to be promising n-type semiconductor candidates for use in organic electronics.
Synthesis of Soluble Fluorene-polyimino Ketone
- Pages: 850-853
- First Published: 06 May 2009

Based on the 9,9-di(4-anilinyl)fluorene, three new fluorene-polyimino ketones have been obtained by the Buchwald-Hartwig cross coupling reaction. Their solubility are improved greatly. They can be dissolved not only in aprotic solvents such as DMSO, DMAc, NMP and DMF, but also in other common organic solvents such as chloroform at room temperature, while they still exhibit excellent thermo stability.