Home | About Journal | Editorial Board | Instruction | Subscribe | Advertisement | Messages Board | Self-test of coincidence rate of papers | Contact Us | Download | 中文
        Office Online
        Journal
Just Accepted
Current Issue
Archive
Advanced Search
Most Read
Most Download
Email Alert
2023 Vol. 31, No. 3
Published: 2023-03-20
 
169
Synthesis, Structure and Photocatalytic Properties of Two Octamolybdate-Based Inorganic-Organic Hybrid Materials
Synthesis, Structure and Photocatalytic Properties of Two Octamolybdate-Based Inorganic-Organic Hybrid Materials[J]. journal1, 2023,31(3): 169-176')" href="#"> TIAN Feng, SHEN Nan, He Mingyang
DOI: 10.15952/j.cnki.cjsc.1005-1511.20020

Two inorganic-organic hybrid materials based on β-[Mo8O26]4−, namely {[Ni(b-Mo8O26)(H2O)4] (H2Fbix) 2H2On (1), {[Co(b-Mo8O26)(H2O)4] (H2Fbix) 2H2O}n (2) (Fbix = 2,3,5,6-tetrafluoro-1,4-bis(imidazol-1-ylmethyl)benzene)) were hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction, power X-ray diffraction, infrared spectroscopy, thermogravimetric analysis and elemental analysis. Single crystal X-ray analysis reveals that 1 and 2 are isostructural. Take 1 as an example, each six-coordinated NiII ion is surrounded by two β-[Mo8O26]4− units and four water molecules, forming an inorganic anionic linear chain. Protonated H2Fbix ligands act as guest and balance the charge of anionic framework. The inorganic chain [Ni(b-Mo8O26)(H2O)4]n2n–, H2Fbix ligand and water guest molecules were further connected by hydrogen bonds to generated the final 3D structure. Both compounds 1 and 2 can serve as heterogeneous catalysts and show good photocatalytic activity for the degradation of MB dye under UV irradiation. Additionally, the catalyst could be easily recovered and reused four times without significantly loss for its crystallinity and activity.
2023 Vol. 31 (3): 169-176 [Abstract] ( 168 ) HTML (1 KB)  PDF (1494 KB)  ( 48 )
177 Preparation and Characterization of a Caspase-3 Targeted PET Molecular Probe
ZHANG Lixia, XU Liang, LI Huirong, LIANG Beibei, LIN Jianguo, QIU Ling
DOI: 10.15952/j.cnki.cjsc.1005-1511.22180
Inducing tumor cell apoptosis is one of the action mechanisms for several antitumor therapies. Therefore, detection of tumor cell apoptosis has become an important index to evaluate the therapeutic effect of tumor. Cell apoptosis-specific molecular probe was designed with caspase-3 as the target, and therapeutic efficacy could be timely evaluated by monitoring the expression level of caspase-3. In this study, a positron emission tomography (PET) probe [18F]8 targeting caspase-3 was reported. The polypeptide and precursor 8 were synthesized by simple solid-phase synthesis method and click chemistry method, respectively. The precursor 8 was labeled with 18F using 18F-19F isotope exchange method to obtain the probe [18F]8 with radiochemical yield of 16% and radiochemical purity of 95%. The probe displayed good stability in PBS and mouse serum, and the lipo-hydro partition coefficient (Log P) of the probe was determined to be -1.69 ± 0.01, suggesting that the probe was hydrophilic. The convenient synthesis method and good physicochemical properties provided a good basis for the application of the probe in PET imaging of tumor apoptosis.
2023 Vol. 31 (3): 177-185 [Abstract] ( 127 ) HTML (1 KB)  PDF (3461 KB)  ( 21 )
186 Synthesis and Cytotoxicity of Two Flavonoids Oxime and Oxime Ether Derivatives
YIN Minhai, LIU Zhiping
DOI: 10.15952/j.cnki.cjsc.1005-1511.22160
Genistein and naringenin are natural active compounds of flavonoids, which have antioxidant, anti-tumor and other biological activities. In this paper, genistein and naringenin were used as the parent materials, and introduced oxime and oxime ether units on the 7-position phenol hydroxyl group of genistein or 4-position carbonyl group of naringenin respectively. Four flavonoid oximes and six oxime ether derivatives were designed and synthesized, and their structures were characterized by 1H NMR and HR-MS spectrometry. MTT assay showed that oxime derivatives were superior to oxime ethers in anti-tumor activity of gastric cancer cell line SGC-7901 in vitro, and compound 3c exhibiting distinct inhibitory against gastric cancer cell line SGC-7901.
2023 Vol. 31 (3): 186-192 [Abstract] ( 129 ) HTML (1 KB)  PDF (1470 KB)  ( 22 )
193 The Syntheses of Cycloalkylaryl Sulfides via Copper-catalyzed C—H bond Activation/C—S
WU Jiahao, WU Yanghao, SONG Shaorui, YANG Yuheng, XU Yingqian, HUANG Ling, CHEN Dingben
DOI: 10.15952/j.cnki.cjsc.1005-1511.22087
In order to design a method of using cheap catalyst to achieve C-H bond activation and construct C—S bond. In this paper, copper-catalyzed C—H bond activation/C—S coupling reaction to synthesize a series of cycloalkylaryl sulfide compounds was studied. A series of cycloalkyl aryl sulfide compounds were synthesized via oxidative denitrogenation C—H bond/C—S coupling procedure using arylsulfonyl hydrazide and cycloalkane as raw materials, CuBr as catalyst, di-tert-butyl peroxide(DTBP) as oxidant, reacted at 120 ℃ for 24 hours. The reaction is suitable for cycloalkanes such as cyclopentane, cyclohexane, cycloheptane, cyclooctane, cyclododecane and aryl hydrazides with different substituent groups(methoxy, nitro, chlorine, methyl). Eighteen aryl sulfide compounds were synthesized with the yields ranging from 41% to 72%. Their structures were characterized by 1H NMR, 13C NMR and HR-MS.
2023 Vol. 31 (3): 193-198 [Abstract] ( 175 ) HTML (1 KB)  PDF (838 KB)  ( 132 )
199 The Structural Determination of the New Psychoactive Substance N-ethylfluamine Hydrochloride
MENG Weining, KONG Fandong, ZHOU Liman,LIANG Shuting, HE Xichao, LI Chenghu,WU Mingxia, HAO Yi, YE Xianwen, SONG Long
DOI: 10.15952/j.cnki.cjsc.1005-1511.22143
A previous unreported new psychoactive substance(NPS) has been abused as a substitute for ketamine and fluamine in some areas of China, recently. Its chemical structure as well as physical and chemical properties are not yet clear. Thus, it is easy to cause missed detections of this NPS in the identification process, posing a serious threat to public health and social security. This study comprehensively used gas chromatography-mass spectrometry(GC-MS), high-resolution mass spectrometry(HR-MS), ultraviolet spectroscopy(UV), infrared spectroscopy(IR) and nuclear magnetic resonance(1H NMR, 13C NMR and 2D-NMR) techniques. combined with inorganic chemical method to determine the structure of the NPS captured in Yulin of Guangxi. The NPS was finally identified as a new compound, N-ethylfluoramine hydrochloride. These results can provide data reference for the detection and identification of the NPS, promote its listing, and reduce the harm to society.
2023 Vol. 31 (3): 199-203 [Abstract] ( 274 ) HTML (1 KB)  PDF (1363 KB)  ( 40 )
204 Synthesis of Novel Maleimide-Pyrazolone-Derived MBH Carbonates by the Morita-Baylis-Hillman Reaction of Pyrazolediones with Maleimides
ZHENG Jinfeng, TANG Xue, PAN Xiaoli, ZHAN Gu, HAN Bo
DOI: 10.15952/j.cnki.cjsc.1005-1511.22024
Morita-Baylis-Hillman (MBH) carbonates are important organic synthetic intermediates. Thus, developing new types of MBH carbonates is of great interest. A Morita-Baylis-Hillman (MBH) reaction of pyrazolediones with maleimides has been developed in the presence of DABCO. Twelve novel maleimide-pyrazolone-derived MBH carbonates were obtained in 40%~87% yields. The structures were characterized by 1H NMR, 13C NMR and HR-MS (ESI).
2023 Vol. 31 (3): 204-209 [Abstract] ( 135 ) HTML (1 KB)  PDF (1419 KB)  ( 77 )
210
Synthesis of Novel Spirooxindole and Spirodihydroqinoline by Domino [3+2] Cycloaddition and Acetylenedicarboxylate Promoted Ring-expansion Reaction
Synthesis of Novel Spirooxindole and Spirodihydroqinoline by Domino [3+2] Cycloaddition and Acetylenedicarboxylate Promoted Ring-expansion Reaction[J]. journal1, 2023,31(3): 210-215')" href="#"> ZHU MeiJun, WU Wentao, HAN Ying, YAN Chaoguo
DOI: 10.15952/j.cnki.cjsc.1005-1511.22043
Multicomponent reaction and domino reaction are widely used in organic synthesis because of their using readily available raw materials, convenient synthetic method, less reaction steps and separation processes. a simple and efficient method for synthesizing spiro compounds via domino reaction was reported in this paper. The one-pot [3+2] cycloaddition reaction of L-thioproline, isatins and chalcones and sequential ring-expansion reaction with dimethyl but-2-ynedioate in refluxing methanol resulted in sulfanyl-containing polycyclic spirooxindole and spirodihydroqinoline derivatives. The spiro compounds were characterized by IR, HR-MS, 1H and 13C NMR spectroscopy and were confirmed by single crystal structures. The formation mechanism of the two compounds included domino ring-opening and annulation process. This reaction has the advantages of using readily available substrates, simple operation and high atomic economy.
2023 Vol. 31 (3): 210-215 [Abstract] ( 97 ) HTML (1 KB)  PDF (2215 KB)  ( 145 )
216 Ruthenium-catalyzed Dehydrogenation of Dihydropyrazines: A Facile Approach to Synthesis Pyrazines
HONG Jianquan, MA Mingyu, CAO Huapeng, FU Yingying, FENG Ruilong, ZHAO Kui, ZHENG Changge
DOI: 10.15952/j.cnki.cjsc.1005-1511.22038
Pyrazines are important heterocyclic compounds, widely used in medicine, organic synthesis and coordination chemistry. Herein, a facile and efficient method for the synthesis of pyrazines is described, where [RuCl2(p-cymene)]2/KOAc catalyzed dehydrogenation of dihydropyrazines to afford various pyrazine derivatives 2a~2p in 43%~90% isolated yields. All of the compounds were confirmed as target compounds by 1H NMR, 13C NMR, IR and elemental analysis.
2023 Vol. 31 (3): 216-221 [Abstract] ( 117 ) HTML (1 KB)  PDF (514 KB)  ( 83 )
222 Synthesis and Photovoltaic Properties of Novel Polythiophene Derivative Containing Thiazoles in Main Chain
SUN Daotong，LI Yuxiang，ZHAO Baofeng, QIN Hongmei
DOI: 10.15952/j.cnki.cjsc.1005-1511.22049
Polythiophene(PT) derivatives are widely used in organic solar cells due to their simple synthesis and good photoelectric properties, but their development is limited by their high energy level. Therefore, in order to reduce its energy level structure, this paper introduced thiazole into the polythiophene derivative backbone chain to synthesize a new polymer donor PBTzCl-T. The photoelectric properties were studied by UV-vis absorption spectroscopy, electrochemical cyclic voltammetry and density functional theory(DFT) calculation. The results show that the introduction of thiazoles can effectively reduce the HOMO and LUMO levels of polymers, thus improving the open circuit voltage of photovoltaic devices. Meanwhile, PBTzCl-T exhibits different preaggregation behaviors in different solvents, which affects the charge transfer ability and active layer morphology of polymer at the interface of D/A, leading to the change of short-circuit current and filling factor of photovoltaic devices.
2023 Vol. 31 (3): 222-229 [Abstract] ( 99 ) HTML (1 KB)  PDF (2871 KB)  ( 109 )
230 Synthesis of N-tryptamine 3-enyl isoindolinone derivatives
LIU Min，LI Wenzhe，Yan Yingkun，CAO Lianyi, LI Min, HUANG Min，Zhang Xiaomei
DOI: 10.15952/j.cnki.cjsc.1005-1511.22047
Isoindoline 1-one has been widely studied in many natural products, pharmaceuticals, and biologically active molecules due to its specific nitrogen containing structural framework. Using o-carboxyacetophenone and tryptamine as starting materials, N-tryptamine 3-alkenylisoindolinone skeleton compound was obtained through two-step dehydration and cyclization under the catalysis of p-toluenesulfonic acid. The operation was simple, and the final target product was obtained in excellent yield(57%~81%). The structure of all products were confirmed by 1H NMR, 13C NMR and HR-MS(ESI).
2023 Vol. 31 (3): 230-237 [Abstract] ( 110 ) HTML (1 KB)  PDF (1883 KB)  ( 31 )
238 Optimization of synthesis process of N-acetyl-L-cysteine
JIN Xin，ZHENG Zhe，QIN Na，ZHENG Hanyun
DOI: 10.15952/j.cnki.cjsc.1005-1511.22114
The synthesis of acetylcysteamine is generally carried out under alkaline conditions. It affects the N-acetyl-L-cysteine’s yield because the raw L-cysteine is unstable under these conditions. we reported the optimized synthesis process of acetylcysteine. The acetylation reaction was carried out under nearly neutral condition, which greatly reduced the generation of inorganic salts, and improved the product quality and yield. The liquid phase purity of acetyl cysteine was 99.89%, the yield was 84.32% and the burning residue was 0.06%. The whole process adhere to the concept of safety, environmental protection, health, the whole process using water as a solvent, with good impurity removal effect, simple operation, mild reaction conditions, good product purity, high yield, suitable for industrial production.
2023 Vol. 31 (3): 238-243 [Abstract] ( 132 ) HTML (1 KB)  PDF (1654 KB)  ( 102 )
Copyright © Editorial Board of Chinese Journal of Synthetic Chemistry
Supported by:Beijing Magtech