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Zhang X.-Y.,Qingdao Agricultural University | Dong D.-Q.,Qingdao Agricultural University | Yue T.,Chemical Technology Academy of Shandong Province | Hao S.-H.,Qingdao Agricultural University | Wang Z.-L.,Qingdao Agricultural University
Tetrahedron Letters | Year: 2014

A novel protocol for acid ionic liquid promoted C(sp3)-H bond functionalization of alkyl azaarenes and nucleophilic addition to aldehydes was developed in good to excellent yields, which provides an efficient approach for the synthesis of alkyl-substituted azaarene derivatives. It is worthwhile to note that acid ionic liquid used for this reaction can be recycled and reused six times without a significant decrease in activity. © 2014 Elsevier Ltd. All rights reserved.


Wei F.,Chemical Technology Academy of Shandong Province | Gao A.-H.,Chemical Technology Academy of Shandong Province | Liu L.-X.,Chemical Technology Academy of Shandong Province
Xiandai Huagong/Modern Chemical Industry | Year: 2012

The new process for preparation of trimethylolpropane diallyl ether is developed using solid sodium hydroxide, trihydroxy methyl propane and allyl chloride as raw materials, and butyl ether as reaction medium and azeotropic dehydrating agent. The key factors affecting the product yield and product quality are controlled and the optimum process conditions are determined. The results show that the high yield of trimethylolpropane diallyl ether can be achieved with less than 8% of ME, more than 90% of DE and less than 1% of TE. The total ether content is greater than 99%. The target product with stable and reliable product quality is obtained with all the indicators better than similar products at home and abroad.


Wang X.,Shandong University | Chi D.,Shandong University | Song D.,Chemical Technology Academy of Shandong Province | Su G.,Shandong University | And 2 more authors.
Journal of Chromatographic Science | Year: 2012

A rapid and highly sensitive high-performance liquid chromatograpy method with fluorescence detection has been developed for determination of glutathione (GSH) in human plasma. A simple pre-column derivatization procedure with 7-flouro-4-nitrobenzo-2-oxa-1,3-diazole (NBD-F) reagent was employed. The separation of the derivatized glutathione was performed using a mobile phase consisting of phosphate buffer (0.02 mol/L, pH 6.0)acetonitrile (77:23, v/v) at a flow rate of 1.0 mL/min with the column temperature 2°C. The eluted derivatives were fluorometrically detected at an excitation wavelength 470 nm and an emission wavelength 530 nm. Under the optimum chromatographic conditions, the calibration curve was linear over the range of 0.1 mol/L to 10.0 mol/L with the correlation coefficient of 0.9988. The precision of the method was satisfactory with the intra-and inter-day coefficient of variation being 6.3, 6.9, respectively. This method has been used to determine glutathione concentrations in plasma samples from healthy individuals. © 2012 The Author.


Xiong Y.,China Pharmaceutical University | Duan H.,China Pharmaceutical University | Meng X.,China Pharmaceutical University | Ding Z.,China Pharmaceutical University | Feng W.,Chemical Technology Academy of Shandong Province
Journal of Chemistry | Year: 2016

Oxychlorination of various phenols is finished in 60 minutes with high efficiency and perfect selectivity under microwave irradiation. These reactions adopt copper(II) chloride (CuCl2) as the catalyst and hydrochloric acid as chlorine source instead of expensive and toxic ones. Oxychlorination of phenols substituted with electron donating groups (methyl, methoxyl, isopropyl, etc.) at ortho- and meta-positions is accomplished with higher conversion rates, lower reaction time, and excellent selectivity. A proposed reaction mechanism is deduced; one electron transfers from CuCl2 to phenol followed by the formation of tautomeric radical that can be rapidly captured by chlorine atom and converts into para-substituted product. © 2016 Yawen Xiong et al.


Yue T.,Chemical Technology Academy of Shandong Province | Gao A.-H.,Chemical Technology Academy of Shandong Province | Wei F.,Chemical Technology Academy of Shandong Province
Xiandai Huagong/Modern Chemical Industry | Year: 2013

A HPLC method is developed for the simultaneous determination of two steps intermediates of homopiperazine, which achieves the objective of middle-controlled analysis. A Shimadzu high performance liquid chromatograph and a VP-ODS C18 column are used for the separation. The mixture of CAN and water (including 25 mmol/L potassium dihydrogen phosphate, adjusting pH to 3.5 with phosphoric acid)=1:1 (V/V) is used as the mobile phase. At a flow rate of 1.0 mL/min, the correlation coefficients of the intermediates are both above 0.999, which are determined by an ultraviolet absorbance detector at 236 nm. Under these conditions, the relative standard deviations are both less than 2.0% and the spiked recoveries are 97%-103%. The experiment results show that this method can reach the requirement of the middle-controlled analysis.


Ji J.,Shandong University | Zhang Y.,Shandong Qianfoshan Hospital | Yang X.-Q.,CDC of Jinan | Jiang R.,Chemical Technology Academy of Shandong Province | And 2 more authors.
Electromagnetic Biology and Medicine | Year: 2012

The increasing use of cellular phones in our society has brought focus on the potential detrimental effects to human health by microwave radiation. The aim of our study was to evaluate the intensity of oxidative stress and the level of neurotransmitters in the brains of fetal rats chronically exposed to cellular phones. The experiment was performed on pregnant rats exposed to different intensities of microwave radiation from cellular phones. Thirty-two pregnant rats were randomly divided into four groups: CG, GL, GM, and GH. CG accepted no microwave radiation, GL group radiated 10 min each time, GM group radiated 30 min, and GH group radiated 60 min. The 3 experimental groups were radiated 3 times a day from the first pregnant day for consecutively 20 days, and on the 21st day, the fetal rats were taken and then the contents of superoxide dismutase (SOD), glutathione peroxidase (GSH-Px), malondialdehyde (MDA), noradrenaline (NE), dopamine (DA), and 5-hydroxyindole acetic acid (5-HT) in the brain were assayed. Compared with CG, there were significant differences (P < 0.05) found in the contents of SOD, GSH-Px, and MDA in GM and GH; the contents of SOD and GSH-Px decreased and the content of MDA increased. The significant content differences of NE and DA were found in fetal rat brains in GL and GH groups, with the GL group increased and the GH group decreased. Through this study, we concluded that receiving a certain period of microwave radiation from cellular phones during pregnancy has certain harm on fetal rat brains. © Informa Healthcare USA, Inc.


Liu M.-L.,Chemical Technology Academy of Shandong Province | Wei F.,Chemical Technology Academy of Shandong Province | Liu L.-X.,Chemical Technology Academy of Shandong Province | Tang X.-C.,Chemical Technology Academy of Shandong Province
Xiandai Huagong/Modern Chemical Industry | Year: 2014

The existing methods for detection of chlorine ion are usually interfered by the reaction between phosphorous acid and silver nitrate, greatly affecting the judgment at the end point of titration. A new detection method for determining the chloride ion in organic phosphonic acid water treatment agent is put forward in this study. It involves the oxidation of residual phosphate in water treatment agent by hydrogen peroxide and the subsequent determination of chloride ion through double salt bridge potentiometric titration. The sudden change of potential, easy judgment of titration end point and acceptable accuracy make it very promising in the determination of chlorine ions.


Li M.-M.,Shandong University | Wang F.-W.,Shandong University | Wang X.-Y.,Chemical Technology Academy of Shandong Province | Zhang T.-T.,Shandong University | And 4 more authors.
Analytica Chimica Acta | Year: 2014

We designed and synthesized a new pyrazoline-based turn-on fluorescence probe for Zn2+ by the reaction of chalcone and thiosemicarbazide. The structure of the probe was characterized by IR, NMR and HRMS spectroscopy. The probe (L) exhibits high selectivity and sensitivity for detecting Zn2+ in buffered EtOH/HEPES solution (EtOH/HEPES=1/1, pH 7.2) with 80-fold fluorescence enhancement, which is superior to previous reports. Job's plot analysis revealed 1:1 stoichiometry between probe L and Zn2+ ions. The association constant estimated by the Benesi-Hildebrand method and the detection limit were 3.92×103M-1 and 5.2×10-7M, respectively. A proposed binding mode was confirmed by 1H NMR titration experiments and density functional theory (DFT) calculations. The probe is cell-permeable and stable at the physiological pH range in biological systems. Because of its fast response to Zn2+, the probe can monitor Zn2+ in living cells. Moreover, the selective binding of L and Zn2+ was reversible with the addition of EDTA in buffered EtOH/HEPES solution and Zn2+ could be imaged in SH-SY5Y neuron cells. © 2014 Elsevier B.V.


Liu J.,China Pharmaceutical University | Meng X.,China Pharmaceutical University | Duan H.,China Pharmaceutical University | Xu T.,Chemical Technology Academy of Shandong Province | And 3 more authors.
Sensors and Actuators, B: Chemical | Year: 2016

Two novel Schiff-base fluorescence probes based on triazole and benzotriazole were designed and synthesized. Corresponding orbital electron distribution and molecular geometry configurations of the compounds were predicted by density functional theory (DFT). Fluorescence properties of probes were detected by UV-vis and fluorescence spectra. Test results indicated that the probes had specific selectivity and high sensitivity for Zn2+ compared with metal ions examined (Ag+, Al3+, Cd2+, Cu2+, Fe3+, Hg2+, K+ and Pb2+). In addition, the detection limit of the probes toward Zn2+ was low down 10-9 M. Therefore, the probes should be potential application in both the environment and biological systems for the detecting of Zn2+. © 2015 Elsevier B.V. All rights reserved.


PubMed | Chemical Technology Academy of Shandong Province and CAS Beijing National Laboratory for Molecular
Type: Journal Article | Journal: The Journal of organic chemistry | Year: 2016

A highly efficient and facile cobalt-catalyzed C-H activation and peroxidation of 2-oxindoles was reported, which provides a new pathway for the synthesis of biologically active 3-peroxy-2-oxindoles from readily available starting materials in excellent chemical yields. The resulting products could be further transformed into various substituted 3-peroxyoxindoles in good to excellent yields. The developed method has been successfully applied to the synthesis of the natural product ()-N-[2-(3-hydroxy-2-oxo-2,3-dihydro-1H-indol-3-yl)ethyl]acetamide.

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