中国化学快报

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Controlling coffee ring structure on hydrophobic polymer surface by manipulating wettability with O₂ plasma

Li-Ying Cui, Yu Yan, Xin-Yu Zhao, Cun-Long Yu, Ying Ma, Bai Yang

中国化学快报. 2017, 28(01): 1-5. https://doi.org/10.1016/j.cclet.2016.07.028

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A simple and novel method is firstly reported for controlling coffee ring structure on polystyrene (PS) film surface by O₂ plasma. O₂ plasma treatment leads to the wettability change of PS surface from hydrophobic to hydrophilic. For hydrophilic PS surface the coffee ring structure is avoided relying on the motion of contact line (CL) while SiO₂ microspheres are left. The motion of the CL is produced based on the viscosity and Marangoni effect with the addition of polymer additives. For hydrophobic PS surface coffee ring structure still persists even with polymer additives because SiO₂ microspheres transfer with the motion of the CL at the beginning of droplet evaporation and accumulate at the droplet edge at late stage with the pinning of the CL. As a result, uniform and macroscale SiO₂ microspheres deposition without coffee ring structure and SiO₂ microspheres deposition with coffee ring structure are controlled by O₂ plasma. This method provides a new way to tune coffee ring structure with smart surface and may be potentially useful for a range of application at material deposition and diagnosing diseases.

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Combining photo-cleavable and hydrogen-abstracting groups in quinoxaline with thioether bond as hybrid photoinitiator

Ji-Yuan Yao, Hong-Hao Hou, Xiao-Dong Ma, Hong-Jie Xu, Zi-Xing Shi, Jie Yin, Xue-Song Jiang

中国化学快报. 2017, 28(01): 6-12. https://doi.org/10.1016/j.cclet.2016.06.008

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We synthesized four diphenylquinoxaline derivatives (SQs) with phenyl-thioether units, which combine photo-cleavable and hydrogen-abstracting groups in one molecule. The photochemistry and photopolymerization of SQs were investigated. SQs possess suitable UV vis absorption in the range of 350 400 nm with high extinction coefficients. UV vis and HPLC-MS spectra revealed that C-S bond in phenyl-thioether group of SQs can be broken by irradiation of UV-light. Photolysis and photopolymerization experiments showed that SQs can be used as photo-cleavable photointiators, their photoinitiating efficiency can be enhanced by hydrogen donor. As photo-cleavable photoinitiators, SQs could initiate hexamethylene diacrylate (HDDA) very efficiently with the double bond conversion (DBC) of 80%. In the presence of ethyl-4-(dimethylamino) benzoate (EDB) as coinitiator, photoinitiator systems initiated photopolymerization of commercial acrylate monomers with higher double bond conversion than 90%. These characteristics make SQs potential photoinitiators in photo-curing field.

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Solution-processed CuO_x as an efficient hole-extraction layer for inverted planar heterojunction perovskite solar cells

Zhi-Kai Yu, Wei-Fei Fu, Wen-Qing Liu, Zhong-Qiang Zhang, Yu-Jing Liu, Jie-Lin Yan, Tao Ye, Wei-Tao Yang, Han-Ying Li, Hong-Zheng Chen

中国化学快报. 2017, 28(01): 13-18. https://doi.org/10.1016/j.cclet.2016.06.021

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A solution-processed CuO_x film has been successfully integrated as the hole-transporting layer (HTL) for inverted planar heterojunction perovskite solar cells (PVSCs). The CuO_x layer is fabricated by simply spin-coating a copper acetylacetonate (Cu(acac)₂) chloroform solution onto ITO glass with high transparency in the visible range. The compact and pinhole-free perovskite film with large grain domains is grown on the CuO_x film. The inverted PVSCs with the structure of ITO/CuO_x/MAPbI₃/PC₆₁BM/ZnO/Al are fabricated and show a best PCE of 17.43% under standard AM 1.5G simulated solar irradiation with a V_OC of 1.03 V, a J_SC of 22.42 mA cm^-2, and a fill factor of 0.76, which is significantly higher and more stable than that fabricated from the often used hole-transporting material PEDOT:PSS (11.98%) under the same experimental conditions. The enhanced performance is attributed to the efficient hole extraction through the CuO_x layer as well as the high-quality CH₃NH₃PbI₃ films grown on the CuO_x. Our results indicate that low-cost and solution-processed CuO_x film is a promising HTL for high performance PVSCs with better stability.

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Preparation and characterization of single crystals[Ln(TBPO)₄(NO₃)₂]NTf₂ (Ln=Eu, Gd)

Chuan-Dong Deng, Yu-Jia Qiao, Qing-De Chen, Xing-Hai Shen

中国化学快报. 2017, 28(01): 19-23. https://doi.org/10.1016/j.cclet.2016.06.020

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Two single crystals[Ln(TBPO)₄(NO₃)₂]NTf₂ (Ln=Eu, Gd) were prepared and characterized by element analysis, single crystal X-ray diffraction, PXRD, FT-IR, TGA and fluorescence spectroscopy. The two compounds have similar coordinate structures, in which the central metal ion is coordinated by four TBPO (Tri-n-butylphosphine oxide) molecules and two bidentate nitrates, while NTf₂^-(bis(trifluor-(bis(trifluoromethylsulfonyl) imide anion) acts as the counter anion. The packing modes of the two crystals are same. The two single crystals are the focus on 8-coordinate tetra-TRPO complexes (TRPO is Trialkyphosphine oxides).

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Observations of carbon-carbon coupling of 4,4-dibromo-pterphenyl on Cu(110) surface at molecular level

Xin-Li Leng, Li-Li Song, Yan Lu, Xiao-Qing Liu, Li Wang

中国化学快报. 2017, 28(01): 24-28. https://doi.org/10.1016/j.cclet.2016.06.036

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The carbon-carbon couplings of 4,4"-dibromo-p-terphenyl (DBTP) on Cu(110) surface have been investigated at a single molecular level by scanning tunneling microscopy. After annealing at 353 K, a mixture of parallel non-organometallic and organometallic intermediates of DBTP molecules along the[1-10] direction of the surface has been observed. Further annealing at 393 K causes one group of molecules to form oligomers with para-para and para-meta motifs via Ullmann reaction and the other group of molecules to synthesize oligomers with meta-meta motifs via direct carbon-carbon coupling reaction. Statistical results directly reveal that the occurrence of reaction type is strongly related to the initial binding configuration of DBTP molecules.

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Sky-blue perovskite light-emitting diodes based on quasi-two-dimensional layered perovskites

Lu Cheng, Yu Cao, Rui Ge, Ying-Qiang Wei, Na-Na Wang, Jian-Pu Wang, Wei Huang

中国化学快报. 2017, 28(01): 29-31. https://doi.org/10.1016/j.cclet.2016.07.001

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A mixed organic (4-phenylbutylamine, 4-PBA) and inorganic (cesium, Cs) cations are used to deposit quasi-two-dimensional layered perovskites. This layered perovskites exhibit good film coverage as twodimensional perovskites and high emission performance close to three-dimensional organic-inorganic hybrid perovskites. Light-emitting diodes (LEDs) are fabricated by using solution process based on the quasi-two-dimensional layered perovskites. The perovskite LEDs exhibit a sky-blue emission with electroluminescence peak at 491 nm and a low turn on voltage at 2.9 V. The maximum external quantum efficiency reaches 0.015% at brightness of 186 cd/m².

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Phenolic constituents from the roots of Alangium chinense

Yan Zhang, Yun-Bao Liu, Yong Li, Shuang-Gang Ma, Li Li, Jing Qu, Dan Zhang, Jian-Dong Jiang, Shi-Shan Yu

中国化学快报. 2017, 28(01): 32-36. https://doi.org/10.1016/j.cclet.2016.05.012

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Three new phenolics (1-3) and twenty-eight known compounds (4-31) were isolated from an ethanolic extract of roots of Alangium chinense. Compound 11 exhibited antiviral activity against Coxsackie virus B3 with IC₅₀ values of 16.89 μmol/L. Compounds 1, 10-17, 19-21, and 23 showed strong antioxidant activity against Fe²⁺-cysteine-induced rat liver microsomal lipid peroxidation, with IC₅₀ values of 0.14-8.18 μmol/L.

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New phenolic compounds from the leaves of Artocarpus heterophyllus

Xiao-Ling Wang, Xia-Xia Di, Tao Shen, Shu-Qi Wang, Xiao-Ning Wang

中国化学快报. 2017, 28(01): 37-40. https://doi.org/10.1016/j.cclet.2016.06.024

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One new 2-arylbenzofuran derivative, artocarstilbene B (1), one new benzaldehyde derivative, (E)-3,5-dihydroxy-4-(3-methylbut-1-enyl) benzaldehyde (2), as well as 18 known compounds (3-20) were obtained from the leaves of Artocarpus heterophyllus. Their structures were elucidated on the basis of extensive spectroscopic techniques including 2D NMR and HR-ESIMS. Many compounds exhibited moderate to weak inhibitory activity against the proliferation of the PC-3, NCI-H460, and A549 cancer cell lines.

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A highly sensitive dopamine sensor based on a polyaniline/reduced graphene oxide/Nafion nanocomposite

Li-Qing Xie, Yan-Hui Zhang, Fei Gao, Quan-An Wu, Piao-Yang Xu, Shan-Shan Wang, Ning-Ning Gao, Qing-Xiang Wang

中国化学快报. 2017, 28(01): 41-48. https://doi.org/10.1016/j.cclet.2016.05.015

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A nanocomposite of polyaniline/reduced graphene oxide (PANI-rGO) was synthesized using a hydrothermal method. The product was characterized by FT-IR, Raman spectra, XRD, SEM and TEM. Then the hybrid material of PANI-rGO and Nafion (PANI-rGO-NF) was prepared and used to modify glassy carbon electrode for the trace determination of dopamine (DA) employing differential pulse voltammetry (DPV). It was found that the hybrid material showed good catalytic activity toward the oxidation of DA, and no response to ascorbic acid (AA) and uric acid (UA) was observed, suggesting a high selectivity of the sensor toward DA. The peak currents were linearly correlated with the concentration of DA in the range from 0.05 μmol/L to 60.0 μmol/L (R=0.996) and 60.0 μmol/L to 180.0 μmol/L (R=0.996) with a detection limit of 0.024 μmol/L (S/N=3). The modified electrode also exhibited excellent repeatability and stability.

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Solid-solid phase transition of (1-C₁₄H₂₉NH₃)₂ZnCl₄ in nanopores of silica gel for thermal energy storage

Qi-Feng Li, Chao Wang, Xiao-Zheng Lan

中国化学快报. 2017, 28(01): 49-54. https://doi.org/10.1016/j.cclet.2016.05.024

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Latent heat storage performance of a layered perovskite-type compound, 1-C₁₄H₂₉NH₃)₂ZnCl₄ (C₁₄Zn), embedded in a series of silica gel (SG) with pore sizes of d=15-200 nm is investigated using differential scanning calorimetry (DSC), and powder X-ray diffractions (XRD). C₁₄Zn in the nanopores of silica gel shows size-dependent phase transition temperature, enthalpy change and supercooling. They have a stable transition temperature and heat capacity at each size in a short-term thermal cycling. Similar Xray diffraction patterns are observed for the nano-sized and the bulk C₁₄Zn. The encapsulation of a phase change material in nanopores is a new way of tuning its thermal energy storage properties for a wider range of temperature regulation.

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Impact of the flexibility of pillar linkers on the structure and CO₂ adsorption property of “pillar-layered” MOFs

Yue-Ling Xu, Qiang Gao, Meng Zhao, Huan-Jun Zhang, Ying-Hui Zhang, Ze Chang

中国化学快报. 2017, 28(01): 55-59. https://doi.org/10.1016/j.cclet.2016.06.006

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A new metal-organic framework {[Zn₂(bpta)(bpy-ee)(H₂O)₂]·x solve}_n (1) (H₄bpta=biphenyl-2,2',6,6'-tetracarboxylic acid and bpy-ee=1,2-bis(4-pyridyl) ethylene) has been obtained under hydrothermal condition, and structurally characterized by single-crystal X-ray diffraction. Complex 1 reveals a threedimensional (3D) "pillar-layered" framework with non-flexible linker, in which some different structure characters can be found compared to that of some related other "pillar-layered" MOFs based on flexible pillar linkers. It demonstrates the impact of the flexibility of pillar linker on the final structure in this system. In addition, the selective CO₂ adsorption performance of 1 was also investigated.

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Concave Pt-Cu-Fe ternary nanocubes:One-pot synthesis and their electrocatalytic activity of methanol and formic acid oxidation

Ying-Xia Wang, Chuan-Fei Liu, Man-Li Yang, Xi-Hui Zhao, Zhi-Xin Xue, Yan-Zhi Xia

中国化学快报. 2017, 28(01): 60-64. https://doi.org/10.1016/j.cclet.2016.05.025

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Concave nanostructures may be developed to improve the specific mass activity of a catalyst for formic acid and methanol electro-oxidation. In this work, we report the elctrocatalytic oxidation of methanol and formic acid in acid medium over concave Pt-Cu-Fe ternary nanocubes (NCs), obtained by the galvanic exchange of Pt and Fe on Cu NCs. The concave Pt-Cu-Fe NCs exhibited improved electrooxidation performance contrasted to Pt-Cu NCs and purchased commercial Pt/C as demonstrated by their improved durability, lower onset potential, and more preferable anti-poisoning properties. These properties are believed to originate from the tailored concave structure of the catalyst and possible synergetic effects among the components of the Pt-Cu-Fe NCs.

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An in situ infrared study of dimethyl carbonate synthesis from carbon dioxide and methanol over well-shaped CeO₂

Shu-Yang Zhao, Sheng-Ping Wang, Yu-Jun Zhao, Xin-Bin Ma

中国化学快报. 2017, 28(01): 65-69. https://doi.org/10.1016/j.cclet.2016.06.003

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The mechanism of dimethyl carbonate (DMC) formation from CO₂ and methanol is investigated using three well-shaped CeO₂ catalysts, nanorod, nanocube and octahedron, which are packed with different crystal planes. In situ Fourier Transform Infrared Spectroscopy (FTIR) is employed to probe each reaction step in the DMC synthesis. The number of -OH groups and the species of CO₂ adsorptions on ceria surface have significant influence on the activity of ceria with different morphologies. Rod-ceria has favorable catalytic activity because of the large amount of -OH groups and the formation of bidentate carbonate species.

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Novel fabrication of copper oxides on AC and its enhanced catalytic performance on oxidative carbonylation of methanol

Ke Shi, Shou-Ying Huang, Zhong-Yao Zhang, Sheng-Ping Wang, Xin-Bin Ma

中国化学快报. 2017, 28(01): 70-74. https://doi.org/10.1016/j.cclet.2016.06.005

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Copper oxides (CuO_x) nanoparticles dispersed on activated carbon (AC) were prepared by using vaporphase methanol as the reducing agent. The CuO_x/AC as prepared exhibited an enhanced catalytic activity in oxidative carbonylation of methanol to dimethyl carbonate (DMC). The catalytic performance was significantly influenced by reduction conditions including temperature and time. With the similar selectivity of DMC, the space time yield (STY) under optimal reduction conditions reached up to 408 mg g^-1 h^-1, which is superior to conventional methods such as thermolysis and solvothermal reduction. Based on the characterization results of XRD, TEM and XPS, the good copper dispersion and high Cu⁺ content obtained by vapor-phase methanol reduction were mainly responsible for the high catalytic activity.

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Preparation of a novel, efficient, and recyclable magnetic catalyst,γ-Fe₂O₃@HAp-Ag nanoparticles, and a solventand halogen-free protocol for the synthesis of coumarin derivatives

Zahra Abbasi, Sobhan Rezayati, Maryam Bagheri, Rahimeh Hajinasiri

中国化学快报. 2017, 28(01): 75-82. https://doi.org/10.1016/j.cclet.2016.06.022

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In this protocol, Ag supported on the hydroxyapatite-core-shell magnetic γ-Fe₂O₃ nanoparticles (γ-Fe₂O₃@HAp-Ag NPs) as a novel, efficient, and magnetically recyclable catalyst is synthesized, and characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and vibrating sample magnetometry (VSM). The use of the catalyst is described in the synthesis of coumarin derivatives by the Pechmann condensation of various phenols with β-ketoesters under solvent-and halogen-free conditions at 80℃. This novel and inexpensive method offers advantages, such as recyclability simple experimental protocol, short reaction time, minimal work-up procedure, and excellent yields of products, together with desirable, eco-friendly, green aspects by avoiding toxic elements and solvents, and ease of recovery from the reaction mixture using an external magnet.

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Triplet excitation dynamics of β-carotene studied in three solvents by ns flash photolysis spectroscopy

Ying Jia, Ying Shi, Peng Wang, Jian-Ping Zhang

中国化学快报. 2017, 28(01): 83-88. https://doi.org/10.1016/j.cclet.2016.05.032

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Upon anthracene-sensitizing, triplet excitation dynamics of β-carotene (β-Car) were studied in n-hexane, in methanol, and in acetonitrile, respectively, by ns flash photolysis spectroscopy. In n-hexane, only the bleaching of the ground state absorption (GSB) and the excitation triplet (³Car^*) absorption were observed, and there were no cationic species detected. In both methanol and acetonitrile, similar excitation dynamics were observed, i.e., ³Car^* having a similar lifetime to that in n-hexane, and the immediate generation of the cation dehydrodimer (^#[Car]₂⁺) upon excitation following transformation into the radical cation Car^·+, since Car^·+ has much longer lifetime in acetonitrile than in methanol. The results prove that both solvent and carotenoid structure determine the triplet excitation mechanism. 2016 Chinese Chemical Society and Institute of Materia Medica, Chinese Academy of Medical Sciences.

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Unusual self-assembled nanoaggregation of the thermally stable metal-free slipped-cofacial J-type phthalocyanine dimer

Alexander Yu. Tolbin, Larisa G. Tomilova

中国化学快报. 2017, 28(01): 89-91. https://doi.org/10.1016/j.cclet.2016.06.038

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Nanoaggregation of the thermally stable bis(2-hydroxy-9(10),16(17),23(24)-tri-tert-butylphthalocyanine) of J-type was observed by the field emission scanning electron microscopy (FE-SEM). Ordered phases, represented as threads composed of about 200 nm diameter circles were discovered, unlike the parent dimeric magnesium complex, in which similar circles combine together to give visually distinguishable zones with widths of about 600 nm and the same distance between them.

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Rhodium catalyzed regioselective arene homologation of aryl urea via double C-H bond activation and migratory insertion of alkyne

Yan Wang, Hao Zhou, Ke Xu, Mei-Hua Shen, Hua-Dong Xu

中国化学快报. 2017, 28(01): 92-96. https://doi.org/10.1016/j.cclet.2016.05.011

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A convenient rhodium catalyzed oxidative arene homologation of aniline derivatives with symmetrical or unsymmetrical alkynes using Cu(OAc)₂ as oxidant is described. Urea group is shown to be effective as a directing group for initial ortho C-H activation. Two migratory insertion events of alkyne into Rh-C bond occur successively, both with complete regioselectivity. This method is particularly useful for synthesis of polyarenes with different substituents, which has not been reported with conventional protocol. A mechanism has been proposed to explain the observed data.

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Novel chiral multidentate P₃N₄-type ligand for asymmetric transfer hydrogenation of aromatic ketones

Meng Tao, Fang Wu, Teng Li, Yan-Yun Li, Jing-Xing Gao

中国化学快报. 2017, 28(01): 97-100. https://doi.org/10.1016/j.cclet.2016.05.028

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Novel chiral multidentate P₃N₄-type ligand has been synthesized and characterized by NMR and HRMS. Using i-PrOH as solvent and hydrogen source, asymmetric transfer hydrogenation of various ketones was investigated. The catalyst generated in situ from chiral multidentate aminophosphine ligand (R,R,R,R)-3 and IrCl(CO)(PPh₃)₂ exhibited highly catalytic activity and excellent enantioselectivity under mild conditions, achieving the corresponding chiral alcohols with up to 99% yield and 99% ee.

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Synthesis of 2,3-dihydroquinazolin-4(1H)-ones catalyzed by α-chymotrypsin

Shi-Guo Zhang, Zong-Bo Xie, Lian-Sheng Liu, Meng Liang, Zhang-Gao Le

中国化学快报. 2017, 28(01): 101-104. https://doi.org/10.1016/j.cclet.2016.06.001

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We discovered that α-chymotrypsin has a promiscuous ability to catalyze the cyclocondensation of aromatic and aliphatic aldehydes with 2-aminobenzamides to afford the corresponding 2,3-dihydroquinazolin-4(1H)-ones successfully in high yields (90%-98%) under alcohol solvent. The catalytic activity of α-chymotrypsin was evaluated through investigating the temperature, the enzyme loading and the ratio of substrates in the enzyme-catalyzed reactions. The present method proves to be efficient and environmentally friendly in terms of short reaction time, high yield, green catalyst and the clean products obtained without further purification processes.

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Synthesis of C8-alkyl-substituted purine analogues by direct alkylation of 8-H purines with tetrahydrofuran catalyzed by CoCl₂·6H₂O

Hong-Ying Niu, Ling-Yun Su, Shi-Xia Bai, Jian-Ping Li, Xi-Lan Feng, Hai-Ming Guo

中国化学快报. 2017, 28(01): 105-108. https://doi.org/10.1016/j.cclet.2016.06.009

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C8-Alkyl-substituted purine analogues were synthesized through direct alkylation of 8-H purine with tetrahydrofuran in the presence of Co catalyst in one step. The reactions gave a series of novel C8-oxygen heterocyclic alkyl purine compounds in good yields under mild reaction conditions by the readily available alkylating reagents, providing a complementary route to the classical coupling reactions for the synthesis of C8-alkyl-substituted purine analogues.

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Practical approach to 2-thioxo-2,3-dihydroquinazolin-4(1H)-one via dithiocarbamate-anthranilic acid reaction

Najmedin Azizi, Mahtab Edrisi

中国化学快报. 2017, 28(01): 109-112. https://doi.org/10.1016/j.cclet.2016.06.012

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A practical and straightforward protocol has been developed for the preparation of 2-thioxo-2,3-dihydroquinazolin-4(1H)-one derivatives from dithiocarbamate chemistry. The method involves the reaction of anthranilic acid derivatives (2-aminobenzoic acid, 2-aminobenzamide and isatoic anhydride) with various dithiocarbamate derivatives using ethanol as solvent. The main advantages of this protocol include practical simplicity, good to high yields, and ease of product isolation, purification and cheapness of the solvent.

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An alternative total synthesis of bolivianine

Jin-Peng Li, Chang-Chun Yuan, Biao Du, Bo Liu

中国化学快报. 2017, 28(01): 113-116. https://doi.org/10.1016/j.cclet.2016.06.013

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An alternative total synthesis of bolivianine in twelve steps is herein reported on the basis of our previous successful bioinspired total synthesis. The present total synthesis features straightforward transformation from an aldol product to the butenolide of the target molecule, and stereoselective DielsAlder cycloaddition to construct ring E, as well as the final spontaneous IMHDA process.

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Synthesis and properties of potassium 5,5'-azobis (1-nitraminotetrazolate): A green primary explosive with superior initiation power

Ya-Nan Li, Bo-Zhou Wang, Yuan-Jie Shu, Lian-Jie Zhai, Sheng-Yong Zhang, Fu-Qiang Bi, Yu-Chuan Li

中国化学快报. 2017, 28(01): 117-120. https://doi.org/10.1016/j.cclet.2016.06.026

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Potassium 5,5'-azobis(1-nitraminotetrazolate), (K₂ABNAT), a new green primary explosive, was synthesized via a safe and convenient synthetic procedure based on methylcarbazate and cyanogen azide. The compound was characterized by single-crystal X-ray diffraction, IR spectroscopy, Raman spectroscopy, multinuclear NMR spectroscopy, elemental analysis, and differential scanning calorimetry (DSC). With the calculated (CBS-4M) heat of formation (617.0 kJ/mol) and the room temperature X-ray density (2.11 g/cm³), impressive values for the detonation parameters such as detonation velocity (8367 m/s) and pressure (31.5 GPa) were computed using the EXPLO5 program. The superior calculated energetic performance show it could serve as a green replacement for the widely used primary explosive, lead(II) azide, which contains toxic ingredient.

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Design, synthesis and insecticidal activities of novel 1-substituted-5-(trifluoromethyl)-1H-pyrazole-4-carboxamide derivatives

Zhi-Bing Wu, Xiang Zhou, Yi-Qiang Ye, Pei-Yi Wang, Song Yang

中国化学快报. 2017, 28(01): 121-125. https://doi.org/10.1016/j.cclet.2016.06.010

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A series of novel 5-(trifluoromethyl)-1H-pyrazole-4-carboxamide derivatives (6a-6n, 7a, 7b, and 8a-8f) were synthesised by placing the amide bond at the 4-position of the pyrazole ring. These derivatives differed from the structure of chlorantraniliprole analogues with the amide bond at the 5-position of the pyrazole ring. Preliminary bioassay results revealed that a few title compounds exhibited good insecticidal activities against lepidopteran pests, such as Plutella xylostella, Mythimna separate, Heliothis armigera, and Ostrinia nubilalis. Some title compounds also elicited broad-spectrum insecticidal activities against dipterous insects including Culex pipiens pallens after altering the amide position. Similar to pyrazole-5-carboxamide analogues, compounds 6b and 6e showed 100% insecticidal activity against P. xylostella, C. pipiens pallens, and M. separate at concentrations of 200, 2, and 200 μg/mL, respectively. This finding suggested that 5-(trifluoromethyl)-1H-pyrazole-4-carboxamide derivatives are potential alternative insecticides for management of agriculture pests.

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Rapid and simultaneous determination of piperidinium and pyrrolidinium ionic liquid cations by ion pair chromatography coupled with direct conductivity detection

Xin-Xin Zhang, Yong-Qiang Liu, Hong Yu, Ren-Qing Zhang

中国化学快报. 2017, 28(01): 126-130. https://doi.org/10.1016/j.cclet.2016.05.034

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A method of ion-pair chromatography with direct conductivity detection was developed on a silicabased monolithic column for the fast and simultaneous determination of piperidinium and pyrrolidinium ionic liquid cations. The effects of the mobile phase, column temperature and flow rate on the retention of the cations were investigated. The retention rules were discussed. As an ion-pair reagent, sodium heptanesulfonate is more suitable than sodium pentanesulfonate for the separation and determination of piperidinium and pyrrolidinium cations. The increase of ion-pair reagent concentration led to the increased retention time of the cations. When acetonitrile content and mobile phase flow were increased, the retention time of the cations became shorter. The retention of piperidinium and pyrrolidinium cations is an exothermic process, and the retention of the cations conforms to the carbon number rule. The chromatographic analysis was performed using the Chromolith Speed ROD RP-18e column, 0.5 μmol/L sodium heptanesulfonate-5% acetonitrile as the mobile phase at a flow rate of 3.0 mL/min and column temperature of 30℃. Separation of N-methyl-N-ethyl piperidinium, N-methyl-N-propyl piperidinium, N-methyl-N-butyl piperidinium and N-methyl-N-ethyl pyrrolidinium, N-methyl-N-propyl pyrrolidinium, N-methyl-N-butyl pyrrolidinium cations were achieved within 10 min. The detection limits (S/N=3) were between 0.19 and 3.08 mg/L. Relative standard deviations (n=5) for peak areas were less than 1.2%. The method has been applied to the determination of piperidinium and pyrrolidinium cations in ionic liquid samples. The spiked recoveries of ionic liquid cations were between 96% and 111%. The method is accurate, reliable, rapid, and has a better practicability.

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An RNA polymerase I-driven human respiratory syncytial virus minigenome as a tool for quantifying virus titers and screening antiviral drug

Yuan-Hui Fu, Ya-Ru Liu, Yan-Peng Zheng, Nan Jiang, Yue-Ying-Jiao, Wei Li, Xiang-Lei Peng, Jin-Sheng He

中国化学快报. 2017, 28(01): 131-135. https://doi.org/10.1016/j.cclet.2016.06.018

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Human respiratory syncytial virus (RSV) is an important pediatric pathogen of lower respiratory tract worldwide. No vaccines and antiviral drugs are available. Herein the use of an RNA polymerase I-driven RSV minigenome for analyzing RSV replication and screening anti-RSV drugs was investigated. The RNA polymerase I (Pol I) was used to transcribe RSV minigenome from the constructed plasmid, designated pHM-RSV-Gluc, of minigenome cDNA which comprised trailer region, gene start sequence (GS), reverse complementary copy of Gaussia luciferase (Gluc) gene, gene end sequence (GE), and leader region in the direction of 5'-3' end and was flanked by promoter and terminator of Pol I. The expression of Gluc was confirmed in pHM-RSV-Gluc transfected HEp-2 cells following RSV infection and had the characteristics of dose-dependent, which provided a rapid, sensitive, and quantitative method for quantifying virus titers and screening antiviral drugs.

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One pot three component synthesis of spiro[indolo-3,10'-indeno[1,2-b] quinolin]-2,4,11'-triones as a new class of antifungal and antimicrobial agents

Kalawati Meena, Sudesh Kumari, Jitender M. Khurana, Amita Malik, Chetan Sharma, Harsh Panwar

中国化学快报. 2017, 28(01): 136-142. https://doi.org/10.1016/j.cclet.2016.06.025

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A simple and efficient three component procedure has been developed for the synthesis of highly substituted spiro[indolo-3,10'-indeno[1,2-b]quinolin]-2,4,11'-triones by one pot three component condensation of enaminones, isatin and indane-1,3-dione in ethanol:water (1:1) in presence of ceric ammonium nitrate (CAN) as catalyst. This method provides several advantages such as lesser reaction time, high yield of products and operational simplicity. The antimicrobial activity of some of the compounds has been investigated against six microbial strains, some of the tested compounds showed good antimicrobial activity.

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Graphene oxide-MnO₂ nanocomposite-modified glassy carbon electrode as an efficient sensor for H₂O₂

Hui-Li Xu, Wei-De Zhang

中国化学快报. 2017, 28(01): 143-148. https://doi.org/10.1016/j.cclet.2016.10.008

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In this study, a new facile preparation method of nanocomposites consisting of graphene oxide and manganese dioxide nanowires (GO/MnO₂ NWs) was developed. The morphology, structure and composition of the resulted products were characterized by transmission electron microscopy, X-ray diffraction and N₂ adsorption and desorption. The GO/MnO₂ nanocomposite was used as an electrode material for non-enzymatic determination of hydrogen peroxide. The proposed sensor exhibits excellent electrocatalytic performance for the determination of hydrogen peroxide in phosphate buffer solution (PBS, pH 7) at an applied potential of 0.75 V. The non-enzymatic biosensor for determination of hydrogen peroxide displayed a wide linear range of 4.90 μmol L^-1-4.50 mmol L^-1 with a correlation coefficient of 0.9992, a low detection limit of 0.48 μmol L^-1 and a high sensitivity of 191.22 μA (mmol L^-1)^-1 cm^-2 (signal/noise, S/N=3). Moreover, the non-enzymatic biosensor shows an excellent selectivity.

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A novel strategy to prepare LDH networks loaded carbon structure by C-MEMS techniques for glucose detection

Bo Hai, Ying-Quan Zou, Gui-Bao Guo, Zheng-De Wang, Yun-Ying Liu, Xiao-Xia Wang, Hui Yan, Li-Tong Ma, Yu-Chen Bai

中国化学快报. 2017, 28(01): 149-152. https://doi.org/10.1016/j.cclet.2016.07.023

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NiAl-layered double hydroxide (NiAl-LDH) networks loaded carbon microcylinder (CMC) hybrid was synthesized for the first time using typical carbon based microelectromechanical systems (C-MEMS) techniques combined with in situ growth progress. The incorporation of NiAl-LDH on C-MEMS structures via a simple pyrolysis of modified photoresist was investigated. With proper control of parameters in lithography and hydrothermal processes, the NiAl-LDH/CMC composites with suitable morphology were fabricated. When the composites applied as new catalytic material for glucose detection, this simple sensor showed satisfying electrocatalytic properties towards glucose oxidation owing to its unique structure and excellent electric conductivity. It is also worth pointing out that this novel fabrication process can equip carbon microfeatures with various nanostructures, and have wide potential applications in scaling up carbon based nanocomposites.

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Enzyme-catalyzed direct three-component aza-Diels-Alder reaction using lipase from Candida sp. 99-125

Dong-Hang Yin, Wei Liu, Zhi-Xiang Wang, Xin Huang, Jing Zhang, De-Chun Huang

中国化学快报. 2017, 28(01): 153-158. https://doi.org/10.1016/j.cclet.2016.10.015

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The direct three-component aza-Diels-Alder reaction was conducted with lipase as a catalyst for the first time. Under the optimized conditions, the aza-Diels-Alder reaction catalyzed by lipase from Candida sp. 99-125 provided the products in moderate to excellent yields. Meanwhile, the endo/exo ratio reached up to 88:12.

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2017年, 第28卷, 第01期　刊出日期：2017-01-22

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2017年, 第28卷, 第01期 刊出日期：2017-01-22

2017年, 第28卷, 第01期　刊出日期：2017-01-22