2-噁唑啉化合物的合成及其在聚合物中的应用

综述了近年来2-噁唑啉化合物在合成领域的研究进展,主要介绍了β-氨基醇与羧酸或羧酸酯反应,酰胺环化反应,以腈类化合物为原料反应等合成方法。总结了2-噁唑啉化合物在聚合物改性方面的应用进展,并预测了2-噁唑啉化合物的合成与应用发展趋势。     

2-甲基-3-丁炔-2-胺的合成工艺研究

以甲基丁炔醇为起始原料合成3-氯-3-甲基-1-丁炔,液氨氨解得到2-甲基-3-丁炔-2-胺,并对合成条件进行了优化,探索出适合工业化生产的2-甲基-3-丁炔-2-胺的合成方法,产物用IR和GC-MS进行表征。     

2-氨基-9,9-二甲基芴的合成与表征

本文对2-氨基-9,9-二甲基芴的合成工艺进行研究。由芴为起始原料,通过选择不同的合成方法,改变反应条件,确定最佳的合成工艺。反应产物通过高效液相色谱检测其纯度,通过核磁共振确定结构,所得产物均与目标化合物相符。     

Synthesis of Azulene Derivatives from 2H-Cyclohepta[b]furan-2-ones as Starting Materials: Their Reactivity and Properties

A variety of synthetic methods have been developed for azulene derivatives due to their potential applications in pharmaceuticals and organic materials. Particularly, 2H-cyclohepta[b]furan-2-one and its derivatives have been frequently used as promising precursors for the synthesis of azulenes. In this review, we describe the development of the synthesis of azulenes by the reaction of 2H-cyclohepta[b]furan-2-ones with olefins, active methylenes, enamines, and silyl enol ethers as well as their reactivity and properties.     

急需开发的医药中间体--2-氰基吡嗪

2-氰基吡嗪是生产治疗结核病药物吡嗪酰胺的重要原料.目前仅日本实现了2-氰基吡嗪的工业化生产,主要生产商是日本的KOEI公司.全球2-氰基吡嗪的年需求量约为2600t,年产量约为1600t,市场缺口达1000t/a.我国生产吡嗪酰胺年需求2-氰基吡嗪600t/a,而其设计能力仅为300t/a,年进口量为480t.国内近几年对2-氰基吡嗪的合成研究较多.文章还对我国2-氰基吡嗪的发展提出了建议.     

The Development of Alkoxide-Directed Metallacycle-Mediated Annulative Cross-Coupling Chemistry

Alkoxide-directed metallacycle-mediated cross-coupling is a rapidly growing area of reaction methodology in organic chemistry. Over the last decade, developments have resulted in more than thirty new and highly selective intermolecular (or “convergent”) C−C bond-forming reactions that have established powerful retrosynthetic relationships in stereoselective synthesis. While early studies were focused on developing transformations that forge a single C−C bond by way of a functionalized and unsaturated metallacyclopentane intermediate, recent advances mark the ability to employ this organometallic intermediate in additional stereoselective transformations. Among these more advanced coupling processes, those that embrace the metallacycle in subsequent [4+2] chemistry have resulted in the realization of a number of highly selective annulative cross-coupling reactions that deliver densely functionalized and angularly substituted carbocycles. This review discusses the early development of this chemistry, recent advances in reaction methodology, and shares a glimpse of the power of these processes in natural product synthesis.     

钛酸镁基微波介质陶瓷粉末制备方法及研究进展

钛酸镁瓷是一种重要的微波介质陶瓷,MgO-TiO2系统存在三种化合物,正钛酸镁、偏钛酸镁、二钛酸镁,三者结构和性能不同。因此为获得高性能陶瓷,通过对组成以及制备工艺的控制,制备单一相的物质至关重要。本文综述了制备钛酸镁粉末的几种方法以及其他几种新兴制备方法。     

水热法制备正交结构层状LiMnO2正极材料的研究进展

层状LiMnO2正极材料的理论容量几乎为尖晶石型锰酸锂（LiMn2O4）的2倍,研究和应用前景广阔.作者较详细的介绍了近年来国内外有关水热法制备层状LiMnO2正极材料的研究工作,评述了由不同锰源制备层状LiMnO2正极材料所存在的优缺点,对今后水热法制备层状LiMnO2正极材料的研究及发展前景进行了展望.     

2-噻吩甲胺类化合物的合成及其应用研究

2-噻吩甲胺是一种重要的药物中间体,由于它及其衍生物具有独特的化学反应活性及生物活性,已被越来越多的研究者所重视。本文对2-噻吩甲胺类化合物合成进展及其典型应用进行了综述,并对各种制备方法进行了分析和概括,为探索一条合理的2-噻吩甲胺制备工艺路线提供相应的参考。     

5-氯-2，3-二氢-2-羟基-1-氧代-1H-茚-2-羧酸甲酯合成研究进展

综述了5-氯-2,3-二氢-2-羟基-1-氧代-1H-茚-2-羧酸甲酯的各种合成方法。认为研究开发基于手性配体的金属催化剂是提高产品ee值和产率的重要发展途径。     

Ni(OH)2与不同碳质材料复合制备超级电容器电极材料研究进展

超级电容器具有功率密度大、寿命长、生产成本低等优点,被认为是最有发展前途的储能系统之一。然而,超级电容器的低能量密度阻碍了其实际应用。由于存储的能量与CV2成正比,可以通过增加材料的电容"C"或操作电压窗口"V"或两者同时增加来提高超级电容器的能量密度。然而具有宽电位窗口的有机电解质离子往往电导率差,成本高,容易引起环境问题。因此为改善能量密度,应采用高比电容的电极材料,故而设计出具有高比电容的适合电极材料就成为研究热点。Ni(OH)2作为超级电容器电极材料,具有理论容量大、成本低、天然丰富、易于合成等优点,近年来备受关注。但由于Ni(OH)2导电率低、比表面积小,其容量劣化严重。碳质材料作为双电层超级电容器的电极材料,其能量存储机制取决于电极表面的电解质离子吸附和解离,具有导电率好、原料丰富、成本较低、电化学稳定性高等优点而应用广泛。因此,有必要将高导电碳质材料引入Ni(OH)2组成复合材料以提高电容性能。笔者综述了Ni(OH)2基材料的合成方法,特别是与碳质材料复合来提高Ni(OH)2基材料的循环稳定性和倍率性能方面的研究新进展。     

The effect of operating conditions on acylation of 2-methylnaphthalene in a microchannel reactor

Acylation of 2-methylnaphthalene(2-MN) is a very important reaction in organic synthesis,and the effiency of the continuous reactor is more than one of the batch reactor.Considering that the Friedel–Crafts acylation is a rapid exothermic reaction,in this study,we perform the acylation of 2-MN in a stainless steel microchannel flow reactor,which is characterized by high mass and heat transfer rates.The effect of reactant ratio,mixing temperature,reaction temperature,and reaction time on product yield and selectivity were investigated.Under the optimal conditions,2-methyl-6-propionylnaphthalene(2,6-MPN) was obtained in 85.8% yield with 87.5% selectivity.Compared with the conventional batch system,the continuous flow microchannel reactor provides a more efficient method for the synthesis of 2,6-MPN.     

发光材料SrAl2O4：Eu2＋的制备及XRD物相分析

采用高温固相法合成SrAl2O4：Eu2＋并用x射线粉末衍射仪进行表征。通过考察合成温度、原料配比的影响,找出了样品的最佳烧结温度及最佳原料配比。     

Direct synthesis of hydrogen peroxide from hydrogen and oxygen: An overview of recent developments in the process

Hydrogen peroxide (H₂O₂) is an important commodity chemical and its demand is growing significantly in the chemical synthesis due to its “green” character. Currently, H₂O₂ is produced almost exclusively by the anthraquinone auto-oxidation (AO) process. The AO process involves indirect oxidation of hydrogen and thus avoids potentially explosive H₂/O₂ mixture. However, this large-scale process presents significant safety issues associated with the transport of bulk H₂O₂. Moreover, the AO process can hardly be considered an environmentally friendly method. In view of this, more economical and environmentally cleaner routes have been explored for the production of H₂O₂. The liquid-phase catalytic direct synthesis of H₂O₂ from H₂ and O₂ offers an attractive green technology for small-scale/on-site production of H₂O₂. However, the direct synthesis process suffers from two major drawbacks: (i) potential hazards associated with H₂/O₂ mixtures and (ii) poor selectivity for H₂O₂ because the catalysts used for H₂O₂ synthesis are also active for its decomposition and hydrogenation to water as well as for H₂ combustion. These serious issues and the recent developments in the direct H₂O₂ synthesis are discussed in this review. The roles of protons (H⁺) and halide ions in promoting the H₂O₂ selectivity are also examined in detail.     

脱水反应生成2-乙烯基吡啶的研究

研究了以2-羟乙基吡啶经脱水生成2-乙烯基吡啶的方法。采用酸碱两类脱水剂,对其反应效果分析比较,发现碱性脱水剂氢氧化钾,更有利于2-乙烯基吡啶合成;探讨了脱水剂用量、反应温度、反应时间等影响因素,得出了适宜的反应条件：n（2-羟乙基吡啶）：n（氢氧化钾）=5：2,在loo。C温度条件下,反应时间2h,反应收率80．2％,产物纯度可达98．1％,水分低于1％。     

NaLn(MoO4)2(Ln=La,Nd)纳米粒子的室温形貌控制合成

钼酸稀土钠盐具有吸收峰宽,阀值低,增益效果明显和发光效高等光学特点,因此近年来被广泛的应用于半导体激光泵浦源,发光二极管或固态激光器元件等方面。在本研究中,我们使用微乳液手段和水热手段对钼酸稀土钠盐纳米材料进行了合成,并使用XRD和TEM等测试手段对实验结果进行了表征与分析,通过改变外界反应条件实现了钼酸稀土钠盐的形貌控制合成。     

负载型磷钨杂多酸催化剂合成辛基多苷

本文以负载型杂多酸为催化剂 ,以葡萄糖和正辛醇为原料 ,直接法合成辛基多苷。制备了不同负载量的PW12 /SiO2 催化剂 ,并加入强酸性树脂以进一步提高催化活性。本文考察了负载量及反应温度等因素对葡萄糖转化率的影响 ,确定了最佳的反应条件     

2-(取代乙炔基)苯甲醛衍生物在有机合成中的应用

作为一类具有特殊结构的重要有机合成中间体，2-(取代乙炔基)苯甲醛衍生物的化学结构是由苯环、取代乙炔基和醛基三部分活性基团构成的共轭体系. 因其具有较高的反应活性，而被广泛的用于构建各种具有新颖结构的苯并碳环或苯并杂环类化合物，如苯并碳环化合物、苯并氮杂环化合物、苯并氧杂环化合物、多元苯并杂环化合物等. 本文综述了2-(取代乙炔基)苯甲醛衍生物在有机合成领域的应用，并对其发展前景进行了展望，为今后2-(取代乙炔基)苯甲醛衍生物在有机合成中的应用提供参考.     

胆碱类低共融溶剂在CO2捕集与分离中的应用

胆碱类低共融溶剂是一种新型的离子液体。它不仅具有传统离子液体的优点,还具有价格低廉、低毒、生物可降解等优势。对胆碱类低共融溶剂在CO₂捕集与分离中所涉及的物理性质,如气体的溶解度、CO₂的吸收-解吸、密度、稳定性、黏度和表面张力等进行考察,并分析了胆碱类低共融溶剂的结构对各物性的影响。通过与传统离子液体的对比,胆碱类低共融溶剂在CO₂捕集与分离中的应用具有一定的优势,如CO₂溶解度高,黏度低。然而,胆碱类低共融溶剂在气体的选择性分离、表面张力等的研究还不足,且热稳定性方面还存在瓶颈,因此,其在CO₂捕集和分离中的应用还有待进一步探讨。     

Synthesis of 1- and 2-Chloro-7 H -benz[ de ]anthr-7-one

Chloro-7 H -benz[ de ]anthr-7-ones (chlorobenzanthrones) are useful as starting materials for synthesis of larger polycyclic aromatic compounds by means of condensation. In the synthesis, the position of the chlorine atom is very important because the structure of condensation products strongly depends on it. For this reason, we have synthesized several chlorobenzanthrones. Although 3- and 4-chlorobenzanthrone were prepared by direct chlorination of benzanthrone and by glycerol condensation of 2-chloroanthraquinone, respectively, the synthesis of 1- and 2-chlorobenzanthrone has not yet been successful. In the present study, we attempted to synthesize them by use of the Sandmeyer reaction. First, we nitrated benzanthrone with nitric acid; 1- and 2-nitrobenzanthrone were obtained by nitration in nitrobenzene at 50-60° and in glacial acetic acid at 105-110°, respectively. Then the nitroderivatives were reduced to corresponding aminoderivatives; the reduction was performed with sodium sulfide for 1-nitrobenzanthrone and with hydrogen chloride and tin for 2-nitrobenzanthrone. Finally, chlorination was carried out by use of the Sandmeyer reaction. The products were separated and purified by column-chromatography. The position of chlorination was confirmed by NMR spectroscopy.