中国化学快报

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Palladium-catalyzed Suzuki-Miyaura cross-coupling reaction of organoboronic acids with N-protected 4-iodophenyl alanine linked isoxazoles

E. Rajanarendar, G. Mohan, E. Kalyan Rao, M. Srinivas

中国化学快报. 2009, 20(01): 1-4. https://doi.org/10.1016/j.cclet.2008.10.022

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Suzuki-Miyaura coupling reaction of N-protected 4-iodopheyl alanine isoxazoles with arylboronic acids, catalyzed by palladium, efficiently produce benzyl-N-(4-bipheyl)-2-(3-methyl-5(E)-2-aryl-1-ethenyl-4-isoxazolyl)-amino-2-oxoethyl) carba-mates in good yields. This process is first of its kind to construct carbon-carbon bond formation having biaryl motif on amino acid linked isoxazole moiety.

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Synthesis of phenanthrimidazole from 9,10-phenanthraquinone and aldehydes by molecular iodine as catalyst

Hossein Behmadi, Mina Roshani, Seyed Mahdi Saadati

中国化学快报. 2009, 20(01): 5-8. https://doi.org/10.1016/j.cclet.2008.09.047

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A new, convenient, efficient, and cost-effective one-pot synthesis of 1H-phenanthro[9,10]imidazol-2-yl from phenantherenquinone and aldehydes, using molecular iodine as catalyst is described. The present methodology offers several advantages such as excellent yields, simple procedure, shorter reaction times, and the use of inexpensive reagents.

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Convergent synthesis of second generation CCK-functional dendrimers

He Gu, Guo Li, Cheng Lin, Zhang Yu, Jiang Bo

中国化学快报. 2009, 20(01): 9-12. https://doi.org/10.1016/j.cclet.2008.10.018

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This paper describes the facile synthesis and characterization of novel dendrimers bearing 9 and 12 CCK peptide fragments on the surface by a convergent method. The structures of dendrimers are characterized by NMR and MS spectrum.

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Synthesis of a novel calix[4]arene-based fluorescent ionophore and its metal ions recognition properties

Qiang Peng, Xing Hua Tang

中国化学快报. 2009, 20(01): 13-16. https://doi.org/10.1016/j.cclet.2008.09.062

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A novel fluorescent ionophore derived from calix[4]arene and pyrazoline was designed and synthesized. Its molecular structure was confirmed by ¹H NMR and element analysis. The resulting material shows specific fluorescent behavior toward the Zn²⁺ ion among the other divalent metal ions, such as Co²⁺, Ni²⁺, Cu²⁺. The primary results indicate this ionophore material is a potential material for developing efficient fluorescent Zn²⁺ chemosensors.

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Microwave-assisted synthesis of diaryl or aryl-alkyl sulfones without catalyst

Jiong Zou, Feng Li, Feng Gang Tao

中国化学快报. 2009, 20(01): 17-20. https://doi.org/10.1016/j.cclet.2008.10.017

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The microwave-assisted coupling reaction of electrondeficient aryl halides with sulfinic acid salts through S_NAr-based addition reactions within 5-30 min. No catalysts were required under our conditions.

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Synthesis of binaphthyl bridged chiral bis-corrole

Ping Lian, Hai Yang Liu, Lan Ying Liu, Lei Shi, Huan Feng Jiang, Chi Kwong Chang

中国化学快报. 2009, 20(01): 21-24. https://doi.org/10.1016/j.cclet.2008.10.016

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Chiral bis-corrole 1 and 2 were prepared by reaction of (s)-2,2'-bis(bromomethyl)-1,1'-binaphthyl and 10-(4-hydroxylphenyl)-5,15-bis(pentafluorophenyl)corrole or 10-(3-hydroxylphenyl)-5,15-bis(pentafluorophenyl)corrole in DMF at 60℃ in the presence of anhydrous K₂CO₃ with an isolated yield~8%. Both 1 and 2 exhibit unsymmetrical induced circular dichroism (ICD) in the soret band with positive exciton chirality.

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Microwave-assisted one-pot synthesis of 3-substituted-3,4-dihydrocoumarins via tendem Konevenagel and Hantzsch reactions

Jing Li, Qiang Liu, Rui Guang Xing, Xiao Xia Shen, Zhen Gang Liu, Bo Zhou

中国化学快报. 2009, 20(01): 25-28. https://doi.org/10.1016/j.cclet.2008.10.007

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convenient route for the synthesis of 3,4-dihydrocoumarin derivates from salicylaldehyde derivates and 1,3-dicarbonyl compounds under solvent-free microwave irradiation conditions was described. In this way, a range of compounds was obtained in moderate to good yields in a short reaction time.

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Synthesis and antibacterial activities of pleuromutilin derivatives

Yuan Yuan Zhang, Ke Ping Xu, Dan Ren, Shao Rong Ge, Yu Liang Wang, Yu Zhong Wang

中国化学快报. 2009, 20(01): 29-31. https://doi.org/10.1016/j.cclet.2008.09.009

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Six new pleuromutilin derivatives were designed and synthesized, confirmed by MS, IR and ¹H NMR techniques. And the antibacterial activities were primarily evaluated in vitro. The results indicated that most of the derivatives showed more potent activities against corresponding bacterial strains than that of pleuromutilin. Especially, compounds 4d and 5b had obvious activities against salmonella compared with pleuromutilin.

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Novel, efficient, and green procedure for the synthesis of 1,5-benzodiazepines catalyzed by MgBr₂ in aqueous media

Shivaji S. Pawar, Murlidhar S. Shingare, Shivaji N. Thore

中国化学快报. 2009, 20(01): 32-36. https://doi.org/10.1016/j.cclet.2008.10.015

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MgBr₂ performs as a novel catalyst for the synthesis of various 1,5-benzodiazepine derivatives from wide range of substituted o-phenylenediamines and various ketones in good to excellent isolated yields (93-98%) using water as solvent at ambient temperature. Several solvents were examined for this reaction; however, in terms of reaction yield and time, water was found to be the optimum solvent. The remarkable advantages offered by this method are easily and inexpensive available catalyst, simple procedure, mild conditions, much faster (40-60 min) reactions and good to excellent yields of products.

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Microwave promoted one-pot synthesis of 3-(2'-amino-3'-cyano-4'-arylpyrid-6'-yl) coumarins

Jian Feng Zhou, Gui Xia Gong, Feng Xia Zhu, San Jun Zhi

中国化学快报. 2009, 20(01): 37-39. https://doi.org/10.1016/j.cclet.2008.10.006

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A facile procedure for the synthesis of 3-(2'-amino-3'-cyano-4'-arylpyrid-6'-yl) coumarins are being reported starting from 3-acetylcoumarin, aromatic aldehydes and malononitrile. The reactions were carried out on microwave irradiation in good yield with short time and easy work-up. The structures of all the compounds have been confirmed on the basis of their analytical, IR, ¹H NMR,and mass spectral data.

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In(OTf)₃ catalyzed allylation reaction of imines with tetraallyltin

Xiao Ning Wei, Ling Yan Liu, Bing Wang, Wei Xing Chang, Jing Li

中国化学快报. 2009, 20(01): 40-43. https://doi.org/10.1016/j.cclet.2008.10.013

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In the presence of catalytic amount of In(OTf)₃ (10 mol%), a series of aldimines reacted with tetraallyltin in a 2:1 molar ratio to afford the corresponding homoallylic amines in good yields. The good atom efficiency was achieved under mild reaction conditions and a new protocol (allyl)₄Sn/In(OTf)₃ for simple imines was developed.

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PEG-400 as an efficient reaction medium for the synthesis of 2,4,5-triaryl-1H-imidazoles and 1,2,4,5-tetraaryl-1H-imidazoles

Xi Cun Wang, Hai Peng Gong, Zheng Jun Quan, Lei Li, He Lin Ye

中国化学快报. 2009, 20(01): 44-47. https://doi.org/10.1016/j.cclet.2008.10.005

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An efficient protocol for the one-pot multicomponent synthesis of various 2,4,5-triaryl-1H-imidazoles and 1,2,4,5-tetraaryl-1H-imidazoles using PEG-400 as reaction medium is described. This method has the advantages of good yields, less pollution and simple reaction conditions.

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One-pot synthesis of (Z)-4-(2-bromovinyl)benezenesulfonamides by microwave-induced simultaneous debrominative decarboxylation and sulfamation of anti-2,3-dibromo-3-(4-hlorosulfonylphenyl)propanoic acid

Wen Sheng Zhang, Chun Xiang Kuang, Qing Yang

中国化学快报. 2009, 20(01): 48-51. https://doi.org/10.1016/j.cclet.2008.10.004

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One-pot simultaneous debrominative decarboxylation and sulfamation of anti-2,3-dibromo-3-(4-chlorosulfonylphenyl)propanoic acid in DMF (for alkyl amines) or DMF-pyridine (for aryl amines) using a diverse range of alkyl and aryl amines under microwave irradiation condition stereoselectively afforded (Z)-4-(2-bromovinyl)benzenesulfonamides in good yields.

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One-pot synthesis of 7-bromo-1-[4-(1-cyano-1-methylethyl)]-phenyl-[1,2,4]-triazole-[4,3-a]-quinoxalin

Yan Yang, Hong Gang Hu, Qing Jie Zhao, Shi Chong Yu, Zhi Gang Dan, Yan Zou, Qiu Ye Wu

中国化学快报. 2009, 20(01): 52-54. https://doi.org/10.1016/j.cclet.2008.10.019

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[1,2,4]-Triazole-[4,3-a]-quinoxaline is an important component of many drugs. The yield of the reported methods for triazole cyclization step was usually as low as 20%. In this article, the triazole cyclization step was successfully done by using microwave method with a high yield of 75% for the first time.

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Solvent-free synthesis of some ethyl arylglyoxylates

Ji Ming Xiang, Bao Lin Li

中国化学快报. 2009, 20(01): 55-57. https://doi.org/10.1016/j.cclet.2008.10.003

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An efficient and convenient approach to synthesize of ethyl arylglyoxylates by solvent-free grinding was described. Eight ethyl arylglyoxylates had been synthesized by this method, this method provided several advantages such as little pollution, high yield,good selectivity, and simple workup procedure, their structures were confirmed by IR, ¹HNMR.

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Polydentate cyclotriphosphazene ligands: Design,synthesis and bioactivity

Le Wang, Yong Ye, Shang Bin Zhong, Yu Fen Zhao

中国化学快报. 2009, 20(01): 58-61. https://doi.org/10.1016/j.cclet.2008.10.020

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Five multinuclear cyclotriphosphazene ligands were synthesized and tested for their cleavage activities to plasmid DNA. All of these new compounds were confirmed by MS, ¹H NMR, ³¹P NMR, ¹³C NMR and IR. Preliminary studies on the cleavage of pUC19 DNA in the presence of metal complexes were performed. The results revealed that these complexes could act as powerful catalysts under physiological conditions. The complexes 3b+Cu can effectively cleave DNA to nicked form, giving hydrolysis rate constant of 0.08/h under physiological conditions. An acid-base catalyzed DNA phosphate-diester hydrolysis mechanism was also proposed.

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A novel ionic liquid based on small size cation

Qing Hai Cai, Ya Wei Hou, Shen Yi Shi, Bin Lu, Yong Kui Shan

中国化学快报. 2009, 20(01): 62-65. https://doi.org/10.1016/j.cclet.2008.10.008

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An ionic liquid material containing small size cation was synthesized and its composition and structure was determined by FT-IR,¹H NMR, ¹³C NMR and element analysis. However, its physical properties such as melting point, viscosity, conductivity, etc.were measured and the results show that the novel ionic liquid is composed of small cation with highly symmetry and larger anion which is very rare among the reported ionic liquid family.

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Chelerythrine chloride binding of guanosine in aqueous solution

Fan Liu, Jian Bin Zhang, Zheng Fu Zhang, Xiao Yan Zhang, Zuo Peng Du, Xiong Hui Wei

中国化学快报. 2009, 20(01): 66-70. https://doi.org/10.1016/j.cclet.2008.10.023

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In this work, the interaction between chelerythrine (CHE) and guanosine is studied usingUV-vis and fluorescence measurements at various temperatures. The UV-vis spectra show that the increasing guanosine concentrations result in the decreasing absorption intensity and red shift of CHE E absorption band (267 nm). The fluorescence spectra are fitted to linear analysis, yielding a binding constant of 1.04×10⁴ L/mol at 298.15 K of CHE with guanosine. Besides, with △_rH_m^Θ=-8.26 kJ=mol, △_rG_m^Θ=-22.90 kJ=mol,and △_rS_m^Θ=-49.38 J/(molK)the interaction should be entropy-driven and exterothermic.

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Mass spectrometry assisted assignments of binding and cleavage sites of Zn(Ⅱ) complex towards oxidized insulin B chain

Jiang Jiang, Qiong Jie Wu, Xiang Yang Cai, Long Gen Zhu, Wen Ji Wang

中国化学快报. 2009, 20(01): 71-75. https://doi.org/10.1016/j.cclet.2008.09.043

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The electrospray ionization mass spectrometry investigation showed that the binding sites of [ZnL]²⁺, where L is 2-[bis(2-aminoethyl)amino]ethanol, with oxidized insulin B chain are Phe1, His5 and Arg22, which lead to the selective cleavages of the peptide bonds at Phe1-Val2, His5-Leu6, Glu21-Arg22, and Arg22-Gly23 of oxidized insulin B chain.

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Aligned single-walled carbon nanotubes array electrode: Fabrication, characterization and application

Xu Zhi Zhang, Kui Jiao

中国化学快报. 2009, 20(01): 76-78. https://doi.org/10.1016/j.cclet.2008.09.007

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In the presence of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) and N-hydroxysuccinimide (NHS),carboxylic group-functionalized single-walled carbon nanotubes (SWNTs) were assembled vertically on the glassy carbon electrode using ethylenediamine as linking agent to fabricate an aligned electrode (SWNTE). The morphological characteristic was studied with atomic force microscope (AFM) and its electrochemical property was investigated using K₃[Fe(CN)₆] as probe.ssDNA had a sensitive voltammetric response at the SWNTE and the oxidative peak potentials of guanine base and adenine base were 0.608 Vand 0.896 V, respectively. Under the optimal conditions, the DPV peak current of guanine base vs. the concentration of ssDNA was linear in the range of 5.4 μg/L-10.8 μg/L with a detection limit of 1 μg/L (S/N=3).

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Chitosan nanoparticles crosslinked by glycidoxypropyltrimethoxysilane for pH triggered release of protein

Ai Wu Pan, Bei Bei Wu, Jian Min Wu

中国化学快报. 2009, 20(01): 79-83. https://doi.org/10.1016/j.cclet.2008.10.012

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pH-responsive-chitosan nanoparticles for the control release of protein drug were prepared by combining two-step crosslinking method, in which chitosan was subsequently crosslinked by sodium tripolyphosphate (TPP) and glycidoxypropyltrimethoxysilane (GPTMS). Compared with TPP crosslinked chitosan particles, the two-step crosslinked nanoparticles were not only pH-responsive but also more stable in wide pH range. Fluorescein isothiocyanate (FITC) labeled anti-human-IgG antibody was used as a model protein drug for evaluating the control release profile of the nano-carrier. The amount of released antibody increased from 5.6% to 50% when the pH of solution shifted from 7.4 to 6.0. The results suggest the possible application of the nanoparticles as pHresponsive drug delivery materials.

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Determination of ephedrine and codeine in human urine by cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography

Li Jun Li, Si Guang Li, Hai Yan Li, Zhuo Cai, Hao Cheng

中国化学快报. 2009, 20(01): 84-87. https://doi.org/10.1016/j.cclet.2008.10.014

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A sensitive method for the determination of ephedrine and codeine in human urine by capillary electrophoresis (CE) was described. In order to improve the sensitivity, two online concentration techniques including cation-selective exhaustive injection (CSEI) and sweeping micellar electrokinetic chromatography (sweeping-MEKC) were used. Under the optimum conditions, the detection limits (S/N=3) were 0.10 μg/L for ephedrine and 0.80 μg/L for codeine. This method was successfully applied to real urine sample analysis.

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Application of potassium ferricyanide in the spectrophotometric determination of captopril

Shi Lei Wang, Min Wang, Quan Min Li

中国化学快报. 2009, 20(01): 88-91. https://doi.org/10.1016/j.cclet.2008.10.021

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A novel method for the determination of captopril by spectrophotometer is described in this paper. The experiment is based on the fact that Fe(Ⅲ) is reduced to Fe(Ⅱ) by captopril, then the in situ formed Fe(Ⅱ) reacts with potassium ferricyanide to give the soluble prussian blue at pH 4.00, and its maximal adsorption wavelength (λ_max) is 735 nm. Good linear relationship is obtained between the absorbance and the concentration of captopril in the wide range of 0.05-20 μg/mL. The linear regression equation is A=-0.04314+0.11423C (μg/mL) with a correlation coefficient R=0.9998. The detection limit (3σ/k) is 0.04 μg/mL, the molar absorption coefficient is 2.5×10⁴ L/mol cm. By mensurating the absorbance of soluble prussian blue, the indirect determination of captopril can be obtained. This method has been successfully applied to determination of captopril in pharmaceutical samples.Analytical results obtained are satisfactory.

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Improved Cd determination in glasses by laser ablation inductively coupled plasma mass spectrometry using nitrogen as a matrix modifier

Qian Ni, Zhao Chu Hu, Zheng Yu Bao, Ya Feng Zhang

中国化学快报. 2009, 20(01): 92-95. https://doi.org/10.1016/j.cclet.2008.10.001

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The addition of 5-10 mL min^-1 nitrogen to the central channel of plasma in Laser ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) increases the sensitivities of Cd by a factor of 3 and decreases oxide interferences by one order of magnitude, which allows the direct analysis of trace levels of Cd in glass samples. This simple method shows a great potential for the direct determination of Cd in various kinds of samples.

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Effect of rare earths on selective hydrogenation of p-chloronitrobenzene over PtMOx/CNTs catalysts

Xiao Xiang Han, Jian Rong Li, Ren Xian Zhou

中国化学快报. 2009, 20(01): 96-98. https://doi.org/10.1016/j.cclet.2008.09.036

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The effect of rare earths (Sm, Pr, Ce, Nd and La) on the hydrogenation properties of p-chloronitrobenzene (CNB) over Pt/CNTs catalyst was studied in ethanol at 303 K and normal pressure. The results exhibited that the hydrogenation of p-CNB could be carried out over PtMOx/CNTs catalysts. Both catalytic activities and yields of p-chloroaniline (CAN) were all improved. PtCeOx/ CNTs catalyst exhibited the best catalytic activity (TOF was 0.47 s^-1) and the highest yield of p-CAN (97.5 mol%). PtCeOx/CNTs (1.0 wt%) catalyst exhibited good stability on the hydrogenation of p-CNB.

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Magnetic field assisted Fenton reactions for the enhanced degradation of methyl blue

Xiao Long Hao, Lu Yi Zou, Guang Sheng Zhang, Yi Bo Zhang

中国化学快报. 2009, 20(01): 99-101. https://doi.org/10.1016/j.cclet.2008.09.058

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Magnetic field was tentatively introduced into Fenton reactions system for the degradation and discoloration of methyl blue as the represent of organic chemical dye, which was a bio-refractory organic pollutant in industry wastewater. It was found that under optimal Fenton reaction conditions, with the assistant of magnetic field in Fenton reactions, the degradation rate of methyl blue, the decomposition rate of H₂O₂ and the conversion rate of Fe²⁺ were accelerated, the extent of them would be improved by the increase of magnetic field intensity. Meanwhile, the mineralization of methyl blue (COD_cr) was improved by over 10% with magnetic field.

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Effect of preparation methods on Pt/alumina catalysts for the hydrogen iodide catalytic decomposition

Zhi Chao Wang, Lai Jun Wang, Ping Zhang, Song Zhe Chen, Jing Ming Xu, Jing Chen

中国化学快报. 2009, 20(01): 102-105. https://doi.org/10.1016/j.cclet.2008.09.059

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Three kinds of Pt/alumina catalysts were prepared by impregnation-hydrogen reduction, impregnation-hydrazine reduction and electroless plating methods. Their differences in the structures, specific areas and particle sizes were characterized by XRD, BET and TEM, respectively. Furthermore, their catalytic activities for the hydrogen iodide (HI) decomposition were evaluated in a fixed bed reactor. The results show that the catalyst 5%Pt/Al₂O₃ prepared by the electroless plating has the optimum catalytic properties for HI decomposition owing to the high dispersion of the platinum nano-particles (<5 nm) on the alumina supports.

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Synthesis and fluorescence properties of cerium-KMgF₃ through a solvothermal process

Guo Xian Zhu, Yong Da Li, Hong Zhou Lian, Jing Hui Yan, Xing Quan Wang

中国化学快报. 2009, 20(01): 106-110. https://doi.org/10.1016/j.cclet.2008.09.032

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Phosphor of KMgF₃:Ce³⁺ is synthesized through solvothermal method at 180℃ and characterized by means of X-ray powder diffraction (XRD) and environment scanning electron microscopy (ESEM). X-ray photoelectron spectroscopy (XPS) is applied to the study of the energy band structure of KMgF₃:Ce³⁺ and confirms the oxygen content of the product is very low. The fluorescence spectra of the rare-earth ion-doped KMgF₃ is investigated by the fluorescence spectrophotometer. In the emission spectra, there is a broadband emission with a maximum center located at 306 nm arising from d-f transition of Ce³⁺ in the host. This will be useful for ultraviolet tunable lasers.

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Facile preparation of methylcellulose/poly(vinyl alcohol) physical complex hydrogels with tunable thermosensitivity

Nan Nan Geng, Cong Ming Xiao

中国化学快报. 2009, 20(01): 111-114. https://doi.org/10.1016/j.cclet.2008.09.003

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Novel complex hydrogels of methylcellulose (MC) and poly(vinyl alcohol) (PVA) with wide-spectrum thermoresponsivity were prepared via physical and mild process. Thermal phase transition of MC/PVA hydrogels exhibited two forms including sol/sol to gel/sol and sol/gel to gel/gel. The phase transition temperature of MC/PVA solution ranged from 38.7 to 60.6℃ and was able to be adjusted by simply changing the feeding ratios of two components. The interior morphology of MC/PVA gels was examined with fluorescence analysis and scanning electron microscopy analysis, which showed that MC was well dispersed in matrix before and after thermally gelling.

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Preparation and characterization of a mixing soft-segment waterborne polyurethane polymer electrolyte

Feng Wu, Yue Jiao Li, Ren Jie Chen, Shi Chen

中国化学快报. 2009, 20(01): 115-118. https://doi.org/10.1016/j.cclet.2008.09.060

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The mixing soft-segment WPU (waterborne polyurethane) polymer electrolytes were synthesized by using PEO (poly(ethylene oxide)) and PDMS (polydimethylsiloxane) as the soft segments. These polymer electrolytes exhibit good thermal and electrochemical stability. The conductivity of the gel polymer electrolyte is 2.52×10^-3 S/cm at 25℃ with the LiTFSI/(DMC+EC) content of 130%.

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X-ray absorption study of tribofilms from ZDDP and overbased salicylate detergents

Yong Wan, M. Kasrai, G. M. Bancroft

中国化学快报. 2009, 20(01): 119-122. https://doi.org/10.1016/j.cclet.2008.09.061

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The interaction of overbased salicylate detergents with zinc dialkyldithiophosphates (ZDDP) and its effect on the formation of tribofilms under boundary lubrication have been studied by means of X-ray absorption near-edge structure spectroscopy. The results show that addition of metallic detergents to neat ZDDP results in the change of surface chemistry of the tribofilm formed from neat ZDDP. Calcium from detergents is digested in the tribofilm. For the high overbased detergents, the deposit of overbasing agent CaCO₃ in the tribofilm is also observed along with the formation of calcium phosphate in tribofilms.

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Dual template approach for the synthesis of hierarchically mesocellular carbon foams

Ming Xian Liu, Li Hua Gan, Ci Tian, Jian Chun Zhu, Zi Jie Xu, Zhi Xian Hao, Long Wu Chen

中国化学快报. 2009, 20(01): 123-126. https://doi.org/10.1016/j.cclet.2008.10.009

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We demonstrated a simple and effective dual-templating approach for the synthesis of hierarchically mesocellular carbon foams by using nonionic surfactant of sorbitan monooleate and silica colloid particles as sacrificial templates, and resorcinol/ formaldehyde as carbon source. The representative carbon foam has dual mesopore sizes of 4 and 10 nm, and possesses the specific surface area of 580 m²/g and the total pore volume of 0.80 cm³/g.

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2009年, 第20卷, 第01期　刊出日期：2009-01-20

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2009年, 第20卷, 第01期 刊出日期：2009-01-20

2009年, 第20卷, 第01期　刊出日期：2009-01-20