中国化学快报

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Controlled synthesis of multi-shelled transition metal oxide hollow structures through one-pot solution route

Xi Wang, Yi-Jun Yang, Ying Ma, Jian-Nian Yao

中国化学快报. 2013, 24(01): 1-6. https://doi.org/10.1016/j.cclet.2013.01.017

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As one type of promising candidates for environmental and energy-related systems, multi-shelled transition metal oxide hollow structures (MS-TMOHSs) have drawn great scientific and technical interest in the past few years. This article highlights recent advances in one-pot solution synthesis of MSTMOHSs. We begin it with an overview of synthetic strategies that have been exploited to achieve these peculiar structures. We then focus on one-pot solution approaches in the following four sections:i) soft templates directed growth;ii) Ostwald ripening;iii) controlled etching;and iv) gas bubble assisted growth. After giving a brief discussion on the unique properties and applications of these multi-shelled hollow structures, we conclude this review with the general challenges and the potential future directions of this exciting area of research.

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A scalable synthesis of 1-amino-5-cyanonaphthalene, a precursor for a nitric oxide probe (NO550) designed via the“dye assembly”principle

Yan-Ming Shen, Lin-Lin Song, Xu-Hong Qian, You-Jun Yang

中国化学快报. 2013, 24(01): 7-8. https://doi.org/10.1016/j.cclet.2013.01.019

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A convenient and scalable synthesis of 1-amino-5-cyanonaphthalene was described.

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Optical monitoring the degradation of PLGA inverse opal film

Li-Guo Sun, Zhuo-Ying Xie, Yuan-Jin Zhao, Hong-Mei Wei, Zhong-Ze Gu

中国化学快报. 2013, 24(01): 9-12. https://doi.org/10.1016/j.cclet.2013.01.012

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plantable materials have broad applications in tissue engineering and in vivo sensors. It is essential to know the detailed information of the implantable materials during their degradation. In this paper, we developed a method to monitor the degradation process of a well-used biomaterial, poly(lactide-coglycolide) (PLGA) by taking advantage of inverse opal structure. We found that mass loss, molecular weight and glass transition temperature of PLGA during the degradation process in Hank's artificial body fluid can be in situ monitored by measuring the optical properties of PLGA inverse opal.

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Atropisomerism of diastereomer diribonucleoside phosphotriester

Lu-Xin Na, Xu-Lin Sun, Meng Wang, Kun-Feng Li, Lei Xing, Zhuo Chen, Zhu Guan, Zhen-Jun Yang

中国化学快报. 2013, 24(01): 13-16. https://doi.org/10.1016/j.cclet.2013.01.018

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Linear diribonucleoside phosphotriester is an important intermediate for synthesizing biologically important compounds, such as cyclic bis(3'-5') diguanylic acid (c-di-GMP) and its analogues. Atropisomerism of diastereomers generated by the chiral center of the P atom, which results in the doubling of signals in ³¹P NMR. The data of ³¹P NMR at different temperature are presented, and thereafter the reason is discussed.

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A simple and green route to transparent boron nitride/PVA nanocomposites with significantly improved mechanical and thermal properties

Zhi-Qiang Duan, Yi-Tao Liu, Xu-Ming Xie, Xiong-Ying Ye

中国化学快报. 2013, 24(01): 17-19. https://doi.org/10.1016/j.cclet.2012.12.014

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A simple and green method is developed to prepare hexagonal boron nitride (h-BN)/poly(vinyl alcohol) (PVA) nanocomposites by using water as a common solvent of h-BN nanosheets and PVA. The obtained h-BN/PVA nanocomposites are highly transparent, and have significantly improved mechanical and thermal properties. They may outperform nano-clay and nano-alumina/PVA nanocomposites as flexible optoelectronic devices, optical windows and heat-releasing materials operated in oxidative or corrosive environment.

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Metal complex with terpyrindine derivative ligand as highly selective colorimetric sensor for iron(Ⅲ)

Peng Wang, Taka-aki Okamura, Hong-Ping Zhou, Wei-Yin Sun, Yu-Peng Tian

中国化学快报. 2013, 24(01): 20-22. https://doi.org/10.1016/j.cclet.2012.12.010

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A new metal complex[MnL₂](NO₃)₂·CH₃CN (1) was synthesized by reaction of 4'-4-(1,2,4-triazol-1-yl)-phenyl-2,2':6',2"-terpyridine (L) with manganese nitrate. The structure of the complex was determined by X-ray crystallography. The results of UV-vis studies showed that the complex exhibits colorimetric sensing ability for Fe³⁺, which can be observed by naked eye.

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Effects of aggregation of poly(3-hexylthiophene) in solution on uniaxial alignment of nanofibers during zone casting

Xiang Gao, Jian-Gang Liu, Yue Sun, Ru-Bo Xing, Yan-Chun Han

中国化学快报. 2013, 24(01): 23-27. https://doi.org/10.1016/j.cclet.2013.01.014

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We report on the effects of aggregation of P3HT with ordered conformation in solution on improving the uniaxial alignment of the P3HT nanofibers by zone casting. Two approaches were employed to change the aggregation of P3HT:P3HT blending with coil insulating polymer and ultrasonic oscillating. The insulator polymer (i.e. PS) which has good solubility in the solution would disturb the aggregation of P3HT to prevent the chains entanglement. The ultrasonic oscillation can further improve the P3HT aggregation with ordered conformation in the solution. As a result, the P3HT nanofibers in the film grew much orientedly by zone casting the ultrasonic oscillating P3HT/PS polymer blends solution than the same solvent P3HT solution without ultrasonic oscillating and blending. The P3HT π-π stacking direction is parallel to the alignment direction of the nanofibers. Meanwhile, the P3HT/PS blend ratio and PS molecular weight have influence on the uniaxial alignment of P3HT nanofibers. Only P3HT/PS is 1:1, the P3HT nanofibers oriented well. The low molecular weight PS can make the P3HT nanofibers orient better than that of the high molecular weight.

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Aza-Michael addition reactions between nitroolefins and benzotriazole catalyzed by MCM-41 immobilized heteropoly acids in water

Shao-Lei Xie, Yong-Hai Hui, Xiang-Ju Long, Chang-Chun Wang, Zheng-Feng Xie

中国化学快报. 2013, 24(01): 28-30. https://doi.org/10.1016/j.cclet.2012.12.009

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MCM-41 supported heteropoly acids (HPAs) catalysts were synthesized, characterized and their catalytic activity was evaluated in an aza-Michael addition reaction between nitroolefins and benzotriazole in water at room temperature. 50 wt% PW/MCM-41 showed the highest activity (up to 96% yield). The catalyst was used in six consecutive experiments without obvious loss of activity, confirming the success of the anchoring process and the catalyst stability.

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Synthesis and characterization of novel polyimides derived from unsymmetrical diamine:2-Amino-5-[4-(2'-aminophenoxy)phenyl]-thiazole

Xin Zhao, Qing-Fen Geng, Tian-Hong Zhou, Xiang-Hu Gao, Gang Liu

中国化学快报. 2013, 24(01): 31-33. https://doi.org/10.1016/j.cclet.2012.11.013

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A new kind of thiazole-containing unsymmetrical ortho-diamine monomer, 2-amino-5-[4-(2'-aminophenoxy)phenyl]-thiazole (o-AAPPT), was synthesized by four steps, using 4-hydroxyacetophen-one as starting material. A novel thiazole-containing polyimide was prepared from the resulting diamine o-AAPPT with BTDA via a conventional one-step method. The resulting polyimide exhibits excellent solubility, film-forming capability and high thermal and thermo-oxidative stability.

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Nanocrystalline TiO₂-HClO₄:A novel, efficient and recyclable catalyst for the chemoselective N-Boc protection of amines under solvent-free conditions

Farhad Shirini, Seyyed Vahid Atghia, Mojtaba Ghazi Jirdehi

中国化学快报. 2013, 24(01): 34-36. https://doi.org/10.1016/j.cclet.2012.12.005

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Nanocrystalline TiO₂-HClO₄, as newly reported catalyst, has been used as an efficient and reusable catalyst for the chemoselective N-Boc protection of amines. The clean, mild acidity condition, quantitative yields of products, short reaction time and low reaction temperature are attractive features of this reaction. In practice, this method is a combination of a satisfactory synthesis and more significantly easy product isolation and purification.

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Synthesis and anti-tumor activity evaluation of novel podophyllotoxin derivatives

Ting Ai, Shao-Yu Shi, Li-Ting Chen, Ling Li, Bo Cao, Ying Gao, Hong Chen, Jing Zhou

中国化学快报. 2013, 24(01): 37-40. https://doi.org/10.1016/j.cclet.2012.11.016

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In order to investigate the effects on the cytotoxicity of indole-3-oxalylamino podophyllotoxin analogs, seven novel podophyllotoxin derivatives were synthesized. The compounds were tested against Hela, K562 or K562/A02 cancer cells in vitro, four of which showed significant cytotoxicity. Among them 9a, 9b and 9c were superior to the positive control VP-16.

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Selective mono-arylation in palladium-catalyzed cross-coupling reaction of dichlorotriazines with phenylboronate ester derivatives

Jin-Fu Dong, Xin Yu, Cheng-Qing Ning, Liang Hu, Nie-Fang Yu

中国化学快报. 2013, 24(01): 41-44. https://doi.org/10.1016/j.cclet.2012.12.004

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Palladium-catalyzed cross-coupling reaction between dichlorotriazines and phenylboronate esters produced the mono-arylated triazines selectively and thus, the corresponding phenyltriazine derivatives could be assembled efficiently in moderate to good overall yields (50-80%).

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Effective synthesis of benzyl halides triggered by in situ prepared hypervalent halides

Xue-Ge Ling, Yan Xiong, Shu-Ting Zhang, Ruo-Feng Huang, Xiao-Hui Zhang

中国化学快报. 2013, 24(01): 45-48. https://doi.org/10.1016/j.cclet.2012.12.013

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An effective approach for the direct benzylhalogenation with in situ generation of hypervalent halides has been developed. A variety of benzyl halides are produced in moderate to excellent yields (up to 99%) with high regioselectivities. UV absorption spectrum is employed to detect the formation of tert-butyl hypoiodite.

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Synthesis and characterization of a tetranuclear copper(Ⅱ) complex with a chiral Schiff base ligand

Hua Xiang, Long Jiang, Huan-Yong Li, Xiao-Dan Zheng, Yu Li

中国化学快报. 2013, 24(01): 49-51. https://doi.org/10.1016/j.cclet.2012.11.011

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The title complex l-[Cu^Ⅱ₄(Hvap)₂(vap)₂(MeOH)₂](ClO₄)₂ 1 has been synthesized and characterized by EA, IR, TGA, solid-state CD spectra and X-ray single-crystal analyses (l-H₂vap:a Schiff base ligand derived from the condensation of o-vanillin and l-2-amino-3-phenyl-1-propanol). Complex 1 crystallizes in monoclinic system, chiral space group P2₁ with a=10.4257(18), b=21.695(4), c=15.721(3)Å, β=94.443(3)°, V=3545.1(11)Å³, Z=2, Cu₄C₇₀H₇₈N₄O₂₂Cl₂, Mr=1652.42, D_c=1.548 g/cm³, F(0 0 0)=1704 and μ(MoKα)=1.338 mm^-1. The final R=0.0682 and wR=0.1420 for 6170 observed reflections with I>2σ(I) and R=0.1775 and wR=0.1830 for all data. The structure of complex 1 contains a boat-shaped {Cu₄O₄} motif. The solid-state CD spectra confirm the chiral nature of complex 1.

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Highly efficient Knoevenagel condensation reactions catalyzed by a proline-functionalized polyacrylonitrile fiber

Guo-Wei Li, Jia Xiao, Wen-Qin Zhang

中国化学快报. 2013, 24(01): 52-54. https://doi.org/10.1016/j.cclet.2012.12.007

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A new proline-functionalized fiber catalyst was employed for the first time to catalyze the Knoevenagel condensation reactions between aromatic aldehydes and ethyl cyanoacetate or malononitrile. This fiber catalyst exhibits a high efficiency (0.5-2 mol% of catalyst with yields of 90%-99%) and excellent reusability (up to 20 times) without the need for additional treatments.

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A new guaianolide from the roots of Pterocypsela elata

Yi-Xiao Bai, Jing Tan, Fu-Lin Yan, Ming-Ming Ding, Xiang Wang

中国化学快报. 2013, 24(01): 55-56. https://doi.org/10.1016/j.cclet.2012.12.015

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In order to find more biologically active substances, we have carefully investigated the chemical constituents of Pterocypsela elata. One new guaianolide, (4S)-11-methoxycarbonyl-guaiane-1(10),5(6),7(11),8(9)-tetraen-6,12-olide was isolated from the EtOAc extracts of the roots of P. elata. Its structure was elucidated by various spectroscopic methods and confirmed by X-ray crystallographic analysis.

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A novel norsesquiterpene alkaloid from the mushroom-forming fungus Flammulina velutipes

Zhen-Yu Xu, Zhi-Ang Wu, Kai-Shun Bi

中国化学快报. 2013, 24(01): 57-58. https://doi.org/10.1016/j.cclet.2012.11.012

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A new norsesquiterpe alkaloid (1) was isolated from the solid culture of mushroom-forming fungus Flammulina velutipes fermented on rice. The structure of 1 was elucidated by spectroscopic methods. The absolute configuration of C-1 in 1 was determined using the circular dichroism data of their[Rh₂(OCOCF₃)₄] complex.

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Behavior of adsorbed diphenyl-sulfide on the Pd/C catalyst for o-chloronitrobenzene hydrogenation

Chang Su, Xiao-Nian Li, Qun-Feng Zhang, Lei Ma, Chun-Shan Lu, Feng Feng

中国化学快报. 2013, 24(01): 59-62. https://doi.org/10.1016/j.cclet.2012.12.006

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A series of diphenyl-sulfide (Ph₂S)-immobilized Pd/C catalysts (Pd-Ph₂S_(x)/C) were prepared using the wetness-impregnation and immobilization method. Pd-Ph₂S_(x)/C catalysts employed for the hydrogenation of o-chloronitrobenzene showed very high selectivity. The structure of Pd-Ph₂S_(x)/C with different molar ratio of ligand (x-values) was characterized by XPS and TG-DSC-MS. The results suggest a "saturated" surface ratio of Ph₂S/Pd (about 0.3) was formed on the Pd-Ph₂S_(x)/C catalysts surface. The Ph₂S immobilized on the Pd particle is quite stable, and the desorption of Ph₂S or dissociative loss of phenyl group was only found at temperatures above 500 K. The possible catalytic mechanism of the Pd-Ph₂S_(x)/C catalyst was also discussed.

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Magnetite/N-doped carboxylate-rich carbon spheres:Synthesis, characterization and visible-light-induced photocatalytic properties

Hong-Jun Tang, Ting-Ting Han, Zhi-Jun Luo, Xiang-Yang Wu

中国化学快报. 2013, 24(01): 63-66. https://doi.org/10.1016/j.cclet.2012.11.015

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A novel magnetically separable visible-light-photocatalyst, magnetite/N-doped carboxylate-rich carbon spheres (N-MCRCSs), was synthesized by a facile ultrasonic method using the magnetite/carboxylaterich carbon spheres (MCRCSs) as precursors. N element has been successfully doped into the MCRCSs in a HNO₃ aqueous solution via an ultrasonic treatment, which were demonstrated by the FT-IR and XPS. NMCRCSs exhibit more intensive absorption over MCRCSs in the entire UV and visible region. N-MCRCSs can not only be easily recycled by applying an external magnetic field, but also exhibit powerful visible light photocatalytic activity.

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Near-infrared diffuse reflectance spectroscopy with sample spots and chemometrics for fast determination of bovine serum albumin in micro-volume samples

Cai-Jing Cui, Wen-Sheng Cai, Xue-Guang Shao

中国化学快报. 2013, 24(01): 67-69. https://doi.org/10.1016/j.cclet.2012.12.012

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Near-infrared diffuse reflectance spectroscopy (NIRDRS) has attracted more and more attention in analyzing the components in samples with complex matrices. However, to apply this technique to micro-analysis, there are still some obstacles to overcome such as the low sensitivity and spectral overlapping associated with this approach. A method for fast determination of bovine serum albumin (BSA) in micro-volume samples was studied using NIRDRS with sample spots and chemometric techniques. 10 mL of sample spotted on a filter paper substrate was used for the spectral measurements. Quantitative analysis was obtained by partial least squares (PLS) regression with signal processing and variable selection. The results show that the correlation coefficient (R) between the predicted and the reference concentration is 0.9897 and the recoveries are in the range of 87.4%-114.4% for the validation samples in the concentration range of 0.61-8.10 mg/mL. These results suggest that the method has the potential to quickly measure proteins in micro-volume solutions.

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A new composite polymer electrolyte based on poly(ethyleneoxide)/polysiloxane/BMImTFSI/organomontmorillonite

Yue-Jiao Li, Feng Wu, Hu-Ren Chao, Shi Chen

中国化学快报. 2013, 24(01): 70-72. https://doi.org/10.1016/j.cclet.2012.12.001

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Composite polymer electrolytes based on poly(ethylene oxide)-polysiloxane/1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide/organomontmorillonite (PEO-PDMS/IL/OMMT) were prepared and characterized. Addition of both an ionic liquid and OMMT to the polymer base of PEO-PDMS resulted in an increase in ionic conductivity. At room temperature, the ionic conductivity of sample PPB100-OMMT4 was 2.19×10^-3 S/cm. The composite polymer electrolyte also exhibited high thermal and electrochemical stability and may potentially be applied in lithium batteries.

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Supramolecular assembly of 2,4,5-trifluorobenzoate complex based on weak interactions involving fluorine atoms

Chun-Hua Ge, Rui Zhang, Ping Fan, Xiang-Dong Zhang, Li-Juan Wang, Fang-Fang Wang

中国化学快报. 2013, 24(01): 73-75. https://doi.org/10.1016/j.cclet.2012.11.014

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The complex[Cd(tfbz)₂(phen)]₂ (1) (tfbz=2,4,5-trifluorobenzoate, phen=1,10-phenanthro-line) was synthesized using trifluorobenzoic acid ligand. The single-crystal structure of 1 has been determined by X-ray crystallography. The packing structure is characterized by the formation of an intricate threedimensional supramolecular network that depends on the C-H…F, F…F, F(lp)…π (lp=lone pair) interactions.

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Fabrication of inorganic-organic hybrid based on polyoxometalate SiW₁₀Fe₂ and folate as peroxidases for colorimetric immunoassay of cancer cells

Zhong Sun, Hai-Zhou Bie, Mei-Jie Wei, Jing-Jing Wang, Xu-Guang Mi, Xiao-Hong Wang, Yin Wu

中国化学快报. 2013, 24(01): 76-78. https://doi.org/10.1016/j.cclet.2012.12.002

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Fabrication of folate and iron-substituted polyoxometalate[(FeOH₂)₂SiW₁₀O₃₆] to form nanoparticles (FA-SiWFe₂) has been achieved. This inorganic-organic hybrid possesses intrinsic peroxidase-like activity, which could be used in detection of cancer cells in colorimetric multiplexed immunoassay.

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A“turn-off”luminescence resonance energy transfer aptamer sensor based on near-infrared upconverting NaYF₄:Yb³⁺, Tm³⁺ nanoparticles as donors and gold nanorods as acceptors

Hong-Qi Chen, Juan Xu, Fei Yuan, Yong Wu, Yi-Yan Zhang, Lun Wang

中国化学快报. 2013, 24(01): 79-81. https://doi.org/10.1016/j.cclet.2012.12.008

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Near-infrared upconverting NaYF₄:Yb³⁺, Tm³⁺ nanophosphors modified with poly(acrylic acid) were prepared and characterized by transmission electron microscopy and luminescence spectroscopy. Based on the observed overlap between the emission spectrum of the NaYF₄:Yb³⁺, Tm³⁺ nanophosphors and the absorption spectrum of the gold nanorods, we believe that a new "turn-off" luminescence resonance energy transfer aptamer sensor was constructed for sensing thrombin in near-infrared region.

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Vesicle formation between single-chained cationic surfactants and ribo-oligonucleotides

Hua Li, Xia Guo

中国化学快报. 2013, 24(01): 82-84. https://doi.org/10.1016/j.cclet.2012.11.010

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Recently, we reported that deoxyribo-oligonucleotides could induce single chained cationic surfactant aggregation to form vesicles. In this paper, we will present that ribo-oligonucleotides can also induce vesicle formation, and compared with deoxyribo-oligonucleotides, ribo-oligonucleotides exhibit a higher inductive efficiency.

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A theoretical study on the water-mediated asynchronous addition between urea and formaldehyde

Tao-Hong Li, Xiao-Guang Xie, Guan-Ben Du

中国化学快报. 2013, 24(01): 85-88. https://doi.org/10.1016/j.cclet.2012.12.003

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The reaction between urea and formaldehyde in water solution was theoretically investigated by using B3LYP and MP2 methods. It was found that the addition of the nitrogen atom in urea to the carbonyl group in formaldehyde precedes the proton transfer and the proton migration from water to the carbonyl group occurs before the proton abstraction from the nitrogen. With one or two water molecules involved in the TS, the activation energy barrier is lowered compared to the TS of the mechanism with no water participation. The energy change along the reaction coordinate clearly shows that a zwitterionic-like intermediate does not exist on the PES. The reaction between urea and formaldehyde occurs in a concerted mechanism but with asynchronous characters. This is different from the stepwise mechanism recently found for the amination reactions of formaldehyde.

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2013年, 第24卷, 第01期　刊出日期：2013-01-20

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2013年, 第24卷, 第01期 刊出日期：2013-01-20

2013年, 第24卷, 第01期　刊出日期：2013-01-20