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索法酮有关物质的合成

中国药物化学杂志 2016年第1期26卷 45-48页

作者：梁兴运穆帅范巧云高立国韩学文张晓军王平保河南大学药学院河南开封475000 天津药物研究院有限公司化学制药部天津300193

目的为了加强对索法酮原料药的质量控制,合成索法酮原料中的3种主要杂质。方法以索法酮为起始原料,经酯化反应制得(E)-2-[5-(3-甲基-2-丁烯氧基)-2-[3-[4-(3-甲基-2-丁烯氧基)]苯基]丙烯酰基]乙酸乙酯(杂质A);以2,4-二羟基苯乙酮为起始... 详细信息

目的为了加强对索法酮原料药的质量控制,合成索法酮原料中的3种主要杂质。方法以索法酮为起始原料,经酯化反应制得(E)-2-[5-(3-甲基-2-丁烯氧基)-2-[3-[4-(3-甲基-2-丁烯氧基)]苯基]丙烯酰基]乙酸乙酯(杂质A);以2,4-二羟基苯乙酮为起始原料,经取代、水解反应制得2-[2-乙酰基-5-(3-甲基-2-丁烯氧基)苯氧基]乙酸(杂质B);以2,4-二羟基苯乙酮为起始物,经过取代、羟醛缩合反应制得(E)-1-[2,4-二(3-甲基-2-丁烯氧基)苯基]-3-[4-(3-甲基-2-丁烯氧基)苯基]-2-烯丙酮(杂质C)。结果与结论索法酮3种杂质的结构经~1H-NMR、^(13)C-NMR和HR-MS谱确证;HPLC面积归一化法测定杂质A、B、C的纯度分别为97.2%、96.9%、97.3%。杂质A、B、C可作为索法酮原料药质量控制的对照品。

关键词：索法酮杂质合成质量控制

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阿哌沙班的合成工艺改进研究

现代药物与临床 2017年第12期32卷 2296-2298页

作者：张馨文张村子范巧云张晓军韩学文高立国穆帅天津泰普药品科技发展有限公司天津300193 天津泰普制药有限公司天津300462 天津药物研究院天津300193

目的对阿哌沙班的合成工艺进行改进研究。方法以4,5,6,7-四氢-1-(4-甲氧基苯基)-6-(4-硝基苯基)-7-氧代-1H-吡唑并[3,4-C]吡啶-3-羧酸乙酯为起始原料,通过还原、取代、环合、胺化反应得到阿哌沙班。结果合成了目标化合物阿哌沙班,经MS、... 详细信息

目的对阿哌沙班的合成工艺进行改进研究。方法以4,5,6,7-四氢-1-(4-甲氧基苯基)-6-(4-硝基苯基)-7-氧代-1H-吡唑并[3,4-C]吡啶-3-羧酸乙酯为起始原料,通过还原、取代、环合、胺化反应得到阿哌沙班。结果合成了目标化合物阿哌沙班,经MS、~1H-NMR确证了结构,质量分数为99.2%,本合成工艺的总收率为76.4%。结论该合成工艺改进后操作简单、安全,适合工业化生产。

关键词：阿哌沙班 Xa因子抑制剂 4 5 6 7-四氢-1-(4-甲氧基苯基)-6-(4-硝基苯基)-7-氧代-1H-吡唑并[3 4-C]吡啶-3-羧酸乙酯合成工艺

A N-CoSe/CoSe_(2)-C@Cu hierarchical architecture as a current collector-integrated anode for potassium-ion batteries

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Rare Metals 2024年第8期43卷 3702-3712页

作者： Zi-Jie mu Yan-Jun Gao Wen-shuai Dong Zong-You Li Qing-Yi Song Han-Jiao Huang Li-Dong Xing Jian-Guo Zhang Wei Wang Qi-Yao Yu State Key Laboratory of Explosion Science and Technology School of Mechatronical EngineeringBeijing Institute of TechnologyBeijing 100081China School of Metallurgical and Ecological Engineering University of Science and Technology BeijingBeijing 100083China

The highly reversible insertion/extraction of large-radius K^+into electrode materials remains a tough goal,especially for con version-type ***,we design a current collector-integrated electrode(N-CoSe/CoSe_(2)-C@Cu) as an advanced anode for potassium-ion battery(PIBs).The conductive CoSe/CoSe_(2) heterojunction with rich Se vacancy defects,conductive sp^2 N-doped carbon layer,and the elastic copper foil matrix can greatly accelerate the electron transfer and enhance the structural ***,the well-designed N-CoSe/CoSe_(2)-C@Cu current collector-integrated electrode displays enhanced potassium storage performance with regard to a high capacity(325.1 mAh·g^(-1) at 0.1 A·g^(-1) after 200cycles),an exceptional rate capability(223.5 mAh·g^(-1) at2000 mA·g^(-1)),and an extraordinary long-term cycle stability(a capacity fading of only 0.019% per cycle over1200 cycles at 2000 mA·g^(-1)).Impressively,ex situ scanning electron microscopy(SEM) characterizations prove that the elastic structure of copper foil is merged into the cleverly designed N-CoSe/CoSe_(2)-C@Cu heterostructure,which buffers the deformation of structure and volume and greatly promotes the cycle life during the potassium/depotassium process.

关键词： Potassium-ion battery Integrated collector electrode CoSe CoSe_2 Heterojunction Copper foil matrix N-doped carbon

A novel approach of tight oil reservoirs stimulation based on fracture controlling optimization and design

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Petroleum Exploration and Development 2020年第3期47卷 632-641页

作者： LEI Qun WENG Dingwei GUAN Baoshan mu Lijun XU Yun WANG Zhen GUO Ying LI shuai Research Institute of Petroleum Exploration&Development PetroChinaBeijing 100083China Stimulation Department of National Energy Tight Oil and Gas R&D Center Langfang 065007China First Oil Factory of Changqing Oilfield Company PetroChinaYan’an 716000China

To deal with the stress interference caused by simultaneous propagation of multiple fractures and the wettability reversal and physical property changes of the reservoir caused by fracturing fluid getting in during large-volume fracturing of tight oil reservoirs through a horizontal well, a non-planar 3D fracture growth model was built, wettability reversal characterizing parameters and change of relative permeability curve were introduced to correct the production prediction model of fractured horizontal well, a fracturing design optimization software(Fr Smart) by integrating geological and engineering data was developed, and a fracturing design optimization approach for tight oil reservoirs based on fracture control was worked out. The adaptability of the method was analyzed and the fracture parameters of horizontal wells in tight oil reservoirs were optimized. The simulation results show that fracturing technology based on fracture control is suitable for tight oil reservoirs, and by optimizing fracture parameters, this technology makes it possible to produce the maximum amount of reserves in the well-controlled unit of unconventional reservoirs. The key points of fracturing design optimization based on fracture control include increasing lateral length of and reducing the row spacing between horizontal wells, increasing perforation clusters in one stage to decrease the spacing of neighboring fractures, and also avoiding interference of old and new fracturing wells. Field tests show that this technology can increase single well production and ultimate recovery. Using this technology in developing unconventional resources such as tight oil reservoirs in China will enhance the economics significantly.

关键词： tight oil reservoir stimulation horizontal well fracture controlling fracturing multi-stage and multi-cluster fracturing fracture parameter

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阿哌沙班中3个杂质的合成研究

现代药物与临床 2016年第8期31卷 1125-1128页

作者：范巧云高立国韩学文穆帅王以富梁兴运张晓军闫少杰天津药物研究院天津300193 天津海光药业股份有限公司天津300457 河南大学药学院河南开封475000

目的设计并合成阿哌沙班中的3个杂质。方法以2-氯-2-[2-(4-甲氧基苯基)亚肼基]乙酸乙酯和5,6-二氢-3-(4-吗啉基)-1-[4-(2-氧代-1-哌啶基)苯基]-2(1H)-吡啶酮为起始原料,经过环合和水解反应得到目标化合物1,化合物1分别经过水解和取代反... 详细信息

目的设计并合成阿哌沙班中的3个杂质。方法以2-氯-2-[2-(4-甲氧基苯基)亚肼基]乙酸乙酯和5,6-二氢-3-(4-吗啉基)-1-[4-(2-氧代-1-哌啶基)苯基]-2(1H)-吡啶酮为起始原料,经过环合和水解反应得到目标化合物1,化合物1分别经过水解和取代反应得到目标化合物2和3。结果合成了目标化合物,并利用MS、~1H-NMR和^(13)C-NMR确证了结构:目标化合物1~3的质量分数分别为99.3%、99.1%、99.2%。结论 3个杂质的合成和纯化为阿哌沙班的杂质研究奠定了物质基础。

关键词：阿哌沙班杂质 2-氯-2-[2-(4-甲氧基苯基)亚肼基]乙酸乙酯 5,6-二氢-3-(4-吗啉基)-1-[4-(2-氧代-1-哌啶基)苯基]-2(1H)-吡啶酮

Catalytic oxidation of pentanethiol on basic nitrogen doped carbon hollow spheres derived from waste tires

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Petroleum Science 2022年第4期19卷 1888-1896页

作者： Jing Luo Wen-Feng Zhang Yan-Chen Wei Ji-Xing Liu Chao Wang Yi-Ru Zou Hai-Tao Ju Li-Ping mu Yan-Hong Chao Hong-Bing Ji Wen-shuai Zhu School of Chemistry and Chemical Engineering Jiangsu UniversityZhenjiang212013JiangsuChina School of Materials Science and Engineering Jiangsu UniversityZhenjiang212013JiangsuChina School of the Environment and Safety Engineering Jiangsu UniversityZhenjiang212013JiangsuChina College of Chemical Engineering and Environment State Key Laboratory of Heavy Oil ProcessingChina University of Petroleum-BeijingChangping102249BeijingChina School of Chemistry Sun Yat-Sen UniversityGuangzhou510275GuangdongChina

A series of basic nitrogen doped carbon hollow spheres(p-N-C) catalysts derived from waste tires were prepared by a green, facile and environmental “leavening” strategy for the catalytic oxidation of pentanethiol. Compared to pristine carbon, the p-N-C has a higher surface curvature conducive to the enrichment of substrates, leading to an excellent catalytic performance. This increased surface curvature of p-N-C was fabricated on the synergistic effect of two foaming agents((NH4)2 C2 O4 and NaHCO3), and the released gas also endows the spherical shell of p-N-C with a hierarchical porous structure, promoting the accessibility of active sites with pentanethiol. Pyridine-like and pyrrolic-like nitrogen atoms were investigated as reactive sites on the p-N-C to accelerate the electron transfer from sulfur to active surface oxygen and enhance the adsorption/oxidation process. As a result, the optimal p-N-C catalyst exhibits superior adsorption and oxidation performance(99.9%) of pentanethiol, outperforming the “unleavened”catalyst(20.8%). This work offers a new avenue for the fabrication of highly efficient materials for the desulfurization of fuel.

关键词： Carbon hollow spheres Nitrogen-doping Waste tires Leavening strategy Pentanethiol

Enhancement of T Follicular Helper Cell-Mediated Humoral Immunity Reponses During Development of Experimental Autoimmune Myasthenia Gravis

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Neuroscience Bulletin 2019年第3期35卷 507-518页

作者： Ying-Zhe Cui Si-Ying Qu Lu-Lu Chang Jia-Rui Zhao Lili mu Bo Sun Hu-Lun Li Tong-shuai Zhang Guang-You Wang Qing-Fei Kong Department of Neurobiology Heilongjiang Provincial Key Laboratory of Neurobiology Harbin Medical University

Myasthenia gravis(MG) is a prototypical antibody-mediated neurological autoimmune disease with the involvement of humoral immune responses in its pathogenesis. T follicular helper(Tfh) cells have been implicated in many autoimmune diseases. However, whether and how Tfh cells are involved in MG remain ***, we established and studied a widely-used and approved animal model of human MG, the rat model with acetylcholine receptor alpha(AChRa) subunit(RAChR97–116)-induced experimental autoimmune myasthenia gravis(EAMG). This model presented mild bodyweight loss 10 days after the first immunization(representing the early stage of disease) and more obvious clinical manifestations and body-weight loss 7 days after the second immunization(representing the late stage of disease). AChR-specific pre-Tfh cells and mature Tfh cells were detected in these two stages, respectively. In cocultures of Tfh cells and B cells, the number of IgG2 bsecreting B cells and the level of anti-AChR antibodies in the supernatant were higher in the cultures containing EAMG-derived Tfh cells. In immunohistochemistry and immunofluorescence assays, a substantial number of CD4^+/Bcl-6^+ T cells and a greater number of larger germinal centers were observed in lymph node tissues resected from EAMG rats. Based on these results, wehypothesize that an AChR-specific Tfh cell-mediated humoral immune response contributes to the development of EAMG.

关键词： Follicular helper T cells Experimental autoimmune myasthenia gravis Acetylcholine receptor Germinal center

Means and verification of broadcast technology applied to laser transmission on horizontal link

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Optoelectronics Letters 2019年第4期15卷 277-283页

作者： mu Yi-ning WANG shuai LIU Guo-zhen LIU Chun-yang ZHAO Kai-qiang JIANG Hui-lin ZHU Yan School of Science Changchun University of Science and Technology Changchun 130022 China Space Opto-electronics Institute Changchun University of Science and Technology Changchun 130022 China

At present, there has been great progress in the field of the point-to-point laser communication technology, in other words, the traditional laser communication technology has been advanced day by day. Furthermore, in order to search for an effective means of achieving localized laser broadcasting communication within a limited range, an effective method of horizontal link laser broadcasting communication is presented, and the corresponding verifiable broadcast communication system is designed. In addition, the laser broadcasting is systematically studied by one physical model built at the optimal distribution of optical power. First of all, the theoretical model of laser beam expansion and the theoretical model of parallel light curtain are made comparisons and analyzed from the angle of attenuation of optical power, and the optical power loss model of the parallel light curtain is established as a result. Secondly, combined with the theory of optical imaging transformation based on Gaussian beam, the field distribution of far field of parallel light curtain is simulated by one leading optical and illumination design software and the relation between the filed distribution of far field of light curtain and the distance of transmission is revealed. Finally, the superiority and feasibility of the parallel light curtain theory model are verified by field communication experiments in different information channels.

关键词： broadcast technology applied laser transmission point-to-point laser communication technology

Co single atoms and nanoparticles dispersed on N-doped carbon nanotube as high-performance catalysts for Zn-air batteries

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Rare Metals 2022年第6期41卷 2055-2062页

作者： Jing-Jing Chen shuai Gu Rui Hao Zhen-Yu Wang mu-Qing Li Zhi-Qiang Li Kun Liu Ke-Meng Liao Zhi-Qiang Wang He Huang Ying-Zhi Li Kai-Li Zhang Zhou-Guang Lu Department of Materials Science and Engineering Guangdong Provincial Key Laboratory of Energy Materials for Electric PowerShenzhen Key Laboratory of Interfacial Science and Engineering of MaterialsSouthern University of Science and TechnologyShenzhen 518055China Department of Mechanical Engineering City University of Hong KongHong Kong 999077China

Diminishing the size of active sites in catalysts is promis-ing to improve the kinetics of oxygen reduction reaction(ORR)and reduce the cost of metal-air ***,the facile preparation of high-performance catalysts with nanoscale active sites still suffers from great ***,we report a facile template-free strategy to fabri-cate Co single atoms and nanoparticles dispersed on porous N-doped carbon nanotube(Co-NCNT)by the pyrolysis of the composites of metal-organic complexes and porous carbon *** from the conventional strategy,the precursor metal-organic complexes in this work were prepared under mild conditions and used without complex purification *** with the pristine carbon nanotube,N-doped carbon nanotube with abundant meso-pores contribute to the formation of nanoscale Co sites.

关键词： nanoparticles composites carbon