4-苯甲氧基苯乙酸的合成方法改进

目的 改进4—苯甲氧基苯乙酸的合成方法。方法 以对经基苯乙酸为原料，经一步反应制得目标产物。结果 所得目标化合物质量与文献一致，收率达90％。结论 新的合成方法时间短，后处理简便，收率高，适合于大量制备。     

罗格列酮氧钒配合物的合成及表征

目的:合成罗格列酮氧钒配合物并进行表征。方法:取罗格列酮与五水硫酸氧钒(VOSO4·5H2O)在适当的条件下(溶剂为乙醇,反应pH值为6)合成罗格列酮氧钒配合物,运用核磁共振氢谱和红外光谱等分析方法对配合物的结构进行了初步确证。结果与结论:确证形成了新的化合物即罗格列酮氧钒配合物,配合物中罗格列酮的化学结构未发生变化,其中2个氧钒均与1个罗格列酮和3个水分子结合。     

四-(三氟乙烷氧基)酞菁锌的光物理性质研究

目的 研究2(3),9(10),16(17),23(24)-四(三氟乙烷氧基)酞菁锌(ZnPcF)光物理性质(包括紫外吸收光谱、荧光光谱)和光敏化作用产生的单线态氧量子产率。方法 采用紫外-可见分光光度法和荧光分光光度法分别测定ZnPcF的紫外-可见吸收光谱、荧光光谱;应用9,10-二甲基蒽为捕捉单线态氧的探针,通过测定光敏化过程中探针浓度的变化,计算ZnPcF的单线态氧(¹O₂)量子产率。结果 与酞菁锌(ZnPc)相比,ZnPcF的紫外可见光谱和荧光光谱都有一定程度的红移。ZnPcF的摩尔消光系数(ε)为1.65×10⁴ L·mol^-1·cm^-1,荧光量子产率为0.197,单线态氧量子产率为0.547。结论 ZnPcF有较大的摩尔消光系数、荧光及单线态氧量子产率,有进一步开发其抗肿瘤效果的前景。     

水溶性八取代酞菁锌配合物（ZnPcBPO8Ⅰ8）的合成及光谱性质研究

目的研究水溶性八取代季铵盐酞菁锌配合物的合成和光谱性质。方法以4-溴-5-硝基邻苯二甲腈为原料,与3-羟基吡啶通过亲核取代反应得到4,5-二（3-吡啶氧基）邻苯二甲腈前驱体,此前驱体通过与无水Zn（OAc）2缩合得到相应的八-β-（3-吡啶氧基）酞菁锌配合物ZnPcBPO8,ZnPcBPO8继续与碘甲烷反应转化成水溶性的酞菁配合物ZnPcBPO8I8,测试其紫外光谱和荧光光谱的性质。结果季铵盐ZnPcBPO8I8在DMF中最大吸收波长在673nm,而在荧光光谱中观察到其荧光发射峰的位置随着酞菁浓度的增大波长逐渐红移。ZnPcBPO8I8在水中以聚集体存在,随着体系中乙醇比例的增加,单体的吸收峰逐渐增强,70%乙醇对其解聚能力最好。在不同pH条件下,不同酸碱性对ZnPcBPO8I8单体—聚集体的平衡影响不同：弱酸性pH为5时主要以单体形式存在,在弱碱性pH为9时主要以单体形式存在,而随酸性或碱性逐渐增强,单体含量都随之下降。结论合成得到的八取代酞菁锌配合物水溶性好,在水溶液中单体—聚集体间平衡随不同的条件相互转变。     

四-(三氟乙烷氧基)酞菁锌的光物理性质研究

目的研究2（3）,9（10）,16（17）,23（24）-四（三氟乙烷氧基）酞菁锌（ZnPcF）光物理性质（包括紫外吸收光谱、荧光光谱）和光敏化作用产生的单线态氧量子产率。方法采用紫外-可见分光光度法和荧光分光光度法分别测定ZnPcF的紫外-可见吸收光谱、荧光光谱;应用9,10-二甲基蒽为捕捉单线态氧的探针,通过测定光敏化过程中探针浓度的变化,计算ZnPcF的单线态氧（1O2）量子产率。结果与酞菁锌（ZnPc）相比,ZnPcF的紫外可见光谱和荧光光谱都有一定程度的红移。ZnPcF的摩尔消光系数（ε）为1.65×104 L·mol^-1·cm^-1,荧光量子产率为0.197,单线态氧量子产率为0.547。结论 ZnPcF有较大的摩尔消光系数、荧光及单线态氧量子产率,有进一步开发其抗肿瘤效果的前景。     

木犀草素Cu(II)配合物的合成与结构表征

目的：木犀草素配合物的研究。方法：在无水乙醇溶剂中，通过溶解、回流合成了木犀草素和醋酸铜金属配合物，并通过元素分析、红外光谱、电子光谱和摩尔电导等表征手段，初步确定了配合物的结构。结果：通过分析可以基本得到金属配合物的分子式和结构：M2L2(Ac)4。结论：得到所合成配合物。     

四-(三氟乙烷氧基)空核酞菁的合成与光谱性质研究

目的 合成了一种新的化合物即四-(三氟乙烷氧基)空核酞菁(H₂PcF),并研究其光谱性质。方法 以4-硝基邻苯二腈和三氟乙醇为起始原料,通过亲核取代反应合成4-三氟乙烷氧基邻苯二腈;再利用醇锂法合成H₂PcF,并通过熔点、红外、质谱、元素分析等进行表征;同时研究其光谱性质(包括紫外吸收光谱、荧光光谱)。结果 H₂PcF的合成产率是34.7%,在可见光尤其是光动力治疗窗(600~800 nm)有较强的吸收,且具有很强的荧光性质和较高的荧光量子产率(φ_F=0.29)。结论 H₂PcF具有良好的溶解性和光谱特性,在光电材料或光学治疗方面具有潜在的应用价值。     

7,8-二羟基黄酮及其稀土配合物的合成与表征

目的 寻找具有抗炎、镇痛、抗凝血作用的黄酮金属配合物药物，充分利用内蒙古地区丰富的稀土资源。方法 采用Baker-Venkataraman反应，合成了7，8-二羟基黄酮，该化合物再与几种稀土配合。结果 合成5种未见文献报道的稀土配合物。结论 用改进工艺后的方法合成黄酮，使重排反应收率提高，溶剂成本降低；而且利用具邻苯二酚结构的黄酮作配体合成配合物，为今后开发研制此类化合物提供了参考。     

半甲苯磺酸索拉非尼一水合物的制备及表征

以4-氯-N-甲基吡啶-2-甲酰胺为原料,与对氨基苯酚反应得到4-（4-氨基苯氧基）-N-甲基-2-吡啶甲酰胺,再与4-氯-3-三氟甲基苯基异氰基酸酯缩合得到索拉非尼碱,将其悬浮于乙醇中,加入甲苯磺酸一水合物搅拌升温至80℃,滴加水,降温析晶,得到半甲苯磺酸索拉非尼一水合物。通过研究发现了索拉非尼的新晶型,其稳定性好,结晶度高,适合产业化。     

Synthesis and Characterization of Impurities in the Production Process of Lopinavir

Lopinavir is an antiretroviral drug used for the inhibition of HIV protease. Four related substances of lopinavir were observed during the manufacturing process of lopinavir in the laboratory and they were identified. The present work describes the origin, synthesis, characterization, and control of these related substances.     

Synthesis and Characterization of Compounds Related to Lisinopril

Lisinopril is a drug of the angiotensin-converting enzyme (ACE) inhibitor class that is primarily used in the treatment of hypertension. During the scale-up of the lisinopril process, one unknown impurity was observed and is identified. The present work describes the origin, synthesis, characterization, and control of this impurity. This paper also describes the synthesis and characterization of three other impurities listed in the European Pharmacopoeia 8.4 (Impurity C, D, and F).     

易达拉封的合成及结构鉴定

将苯肼加热至50℃，与丁酮酰胺反应，可直接得到易达拉封，收率达97％。     

氯沙坦合成工艺改造

以2-正丁基-4-氯-1H咪唑-5-甲酰基和对溴苄溴为原料,合成氯沙坦。其间经过烷基化,得到重要中间体2-正丁基-4-氯-1-[4-溴-苯甲基]-1H咪唑-5-甲酰基,再经取代的硼酸偶联、脱保护、硼氢化钠还原得到氯沙坦。此合成路线较为简便。     

The Critical Roles of Zinc: Beyond Impact on Myocardial Signaling

Zinc has been considered as a vital constituent of proteins, including enzymes. Mobile reactive zinc (Zn²⁺) is the key form of zinc involved in signal transductions, which are mainly driven by its binding to proteins or the release of zinc from proteins, possibly via a redox switch. There has been growing evidence of zinc''s critical role in cell signaling, due to its flexible coordination geometry and rapid shifts in protein conformation to perform biological reactions. The importance and complexity of Zn²⁺ activity has been presumed to parallel the degree of calcium''s participation in cellular processes. Whole body and cellular Zn²⁺ levels are largely regulated by metallothioneins (MTs), Zn²⁺ importers (ZIPs), and Zn²⁺ transporters (ZnTs). Numerous proteins involved in signaling pathways, mitochondrial metabolism, and ion channels that play a pivotal role in controlling cardiac contractility are common targets of Zn²⁺. However, these regulatory actions of Zn²⁺ are not limited to the function of the heart, but also extend to numerous other organ systems, such as the central nervous system, immune system, cardiovascular tissue, and secretory glands, such as the pancreas, prostate, and mammary glands. In this review, the regulation of cellular Zn²⁺ levels, Zn²⁺-mediated signal transduction, impacts of Zn²⁺ on ion channels and mitochondrial metabolism, and finally, the implications of Zn²⁺ in health and disease development were outlined to help widen the current understanding of the versatile and complex roles of Zn²⁺.     

Synthesis,characterization and biological activities of Schiff bases derived from 2-hydroxy-3-nitrobenzaldehyde

Four novel Schiff bases were synthesized by the condensation reaction of 2-hydroxyl-3-nitrobenzaldehyde with either benzothiazoles or benzimidazolamines. The compounds 1–4 were characterized by spectroscopic and analytical methods. The crystal structures of 6-methoxy-1,3-benzothiazol-2-amine and compound 2 are reported only. The 6-methoxy-1,3-benzothiazol-2-amine was found to crystallize in the orthorhombic crystal system in the space group Pbca, having eight molecules in the unit cell, while compound 2 was found to crystallize in the monoclinic crystal system in the space group P2₁/c.The biological activities of these compounds were investigated by evaluating their antibacterial, antifungal, antimalarial, anti-HIV and anti-trypanosomiasis activities. These compounds displayed very interesting antibacterial, antifungal, antimalarial, anti-trypanosomiasis, anti-HIV and low cytotoxicity activity against HeLa cells.     

Identification and Characterization of Potential Impurities in Raloxifene Hydrochloride

During the synthesis of the bulk drug Raloxifene hydrochloride, eight impurities were observed, four of which were found to be new. All of the impurities were detected using the gradient high performance liquid chromatographic (HPLC) method, whose area percentages ranged from 0.05 to 0.1%. LCMS was performed to identify the mass number of these impurities, and a systematic study was carried out to characterize them. These impurities were synthesized and characterized by spectral data, subjected to co-injection in HPLC, and were found to be matching with the impurities present in the sample. Based on their spectral data (IR, NMR, and Mass), these impurities were characterized as Raloxifene-N-Oxide [Impurity: 1]; EP impurity A [Impurity: 2]; EP impurity B [Impurity: 3]; Raloxifene Dimer [Impurity: 4]; HABT (6-Acetoxy-2-[4-hydroxyphenyl]-1-benzothiophene or 6-Hydroxy-2-[4-acetoxyphenyl]-1-benzothiophene) [Impurity: 5]; PEBE (Methyl[4-[2-(piperidin-1-yl)ethoxy]]benzoate) [Impurity: 6]; HHBA (1-[6-hydroxy-2-(4-hydroxyphenyl)-1-benzothiophen-3-yl]ethanone) [Impurity: 7]; 7-MARLF (7-Acetyl-[6-hydroxy-2-(4-hydroxyphenyl)-1-benzothiophen-3-yl][4-[2-(piperidin-1-yl)ethoxy]phenyl methanone) [Impurity: 8]; of which impurities 5–8 are reported for the first time.     

羧甲基壳聚糖银、锌、铈的合成及抑菌实验的研究

报道了羧甲基壳聚糖银、锌、铈的合成及其混合物对金黄色葡萄球菌、铜绿假单孢菌、大肠埃希氏菌、肺炎克雷伯氏菌和变形杆菌的抑菌作用 ,并与磺胺嘧啶银进行比较 ,结果发现 ,羧甲基壳聚糖银、锌、铈水溶液 (含量为 0 .6 95mg/ml,Ag、Zn、Ce含量分别为 0 .2 5 2× 10 6、5 .2 8× 10 6、2 .15 4× 10 6)对上述 5种细菌 (含量为10 4CFU/ml)杀菌率为 96 %以上 ,与 1.0mg/ml磺胺嘧啶银作用相当