硅钨杂多酸催化合成戊二酸二异辛酯

戊二酸是一种很有利用价值的化工原料，国外对其开发利用较早，已制成戊二酸二甲酯或乙酯作为溶剂，有的还将戊二酸制成酯类增塑剂，认为戊二酸作为奇碳数二元酸，其增塑性能要优于己二酸酯类［１］。多年来，国内对己二酸生产过程中副产的戊二酸一直没有很好利用［２］。...     

含苯并噻唑杂环的α-氨基膦酸二苯酯的合成及生物活性

α氨基膦酸作为氨基酸的含磷类似物,具有广泛的除草［１］、杀菌［２］和植物生长调节活性［３］．最近的研究表明,某些α氨基膦酸衍生物还具有较好的抗植物病毒活性［４,５］．在研究植物病毒抑制剂的过程中,我们发现含苯并噻唑杂环的α氨基膦酸二乙酯类化合物...     

四羟乙基己二酰胺的合成及应用研究

羟乙基二酰胺是重要的化工产品 ,广泛用于日化、表面活性剂、涂料等领域[1] 。目前合成四羟乙基二酰胺类的方法主要有 :( 1 )二元酸与二乙醇胺直接反应 ,该法得到的是酰胺及酯的混合物。( 2 )采用二元酰胺与环氧乙烷或氯乙醇反应 ,可得到纯度较高的产品。但环氧乙烷沸点低 ,爆炸极限宽 ,操作不便且不安全。 ( 3 )采用二酸酯与二乙醇胺在碱催化下反应是国内外目前使用的主要方法。该法主要的问题是制得的产品纯度不高 ,有较多的三羟乙基及二羟乙基 ,甚至一羟乙基化合物及聚酯等。本文采用中性的锆酸酯为催化剂[2 ] ,将己二酸二酯与二乙醇胺进…     

氨基磺酸对酯化反应的催化作用

氨基磺酸对酯化反应的催化作用张竞清，刘间生（佛山大学化学系佛山５２８０００）关键词氨基磺酸，催化，酯化，乙酸正丁酯氨基磺酸Ｈ２ＮＳＯ３Ｈ是一种高稳定性、不吸湿的固体酸［１］。主要用作金属表面处理剂，合金电镀添加剂，织物染色助剂以及硬表面清洗剂等［２］...     

含氢硅氧烷的硅氢加成反应

含氢硅氧烷的硅氢加成反应师彤，谢择民，王清正（中国科学院化学研究所北京１０００８０）关键词含氢硅氧烷，二乙烯基四甲基二硅氧烷，硅氢加成反应，~1ＨＮＭＲ铂催化硅氢加成的机理~［１，２］、副反应￣［３，４］、聚合物性能￣［３，５］等均有报道，个别文献用粘?..     

双■唑啉化合物偶联聚酯的研究Ⅱ.聚对苯二甲酸乙二酯的偶联反应

用特性粘度（［η］）和羧值为参数，研究了双唑啉化合物（ＢＯＺ）对聚对苯二甲酸乙二酯（ＰＥＴ）的扩链反应动力学过程，表明ＢＯＺ是与ＰＥＴ中羧基反应，考察了不同工艺生产的ＰＥＴ的扩链效果，结果说明达到的［η］极大值取决于原始ＰＥＴ的［η］与羧值之比     

高效液相色谱法测定邻氰基苄基膦酸二乙酯

高效液相色谱法测定邻氰基苄基膦酸二乙酯＊许峰何大森宋跃群张禹应玲（浙江师范大学化学系浙江金华３２１００４）关键词高效液相色谱邻氰基苄基膦酸二乙酯邻氰基苄基膦酸二乙酯（ＤＣＰ）是生产荧光增白剂ＥＲ的重要中间体［１］。它由邻氰基甲苯光氯化，邻氰基氯苄酯化...     

二苄基一氯化锡二硫代氨基甲酸酯的合成

二烃基氯化锡及其衍生物具有较强的抗癌活性，日益受到人们的重视。关于含有Ｓｎ—Ｏ键的二烃基锡衍生物的合成研究已有大量报道［１］。但含Ｓｎ—Ｓ键二烃基锡衍生物的合成研究则较少［２］，而二烃基一氯化锡二硫代氨基甲酸酯的合成研究尚未见报道。为了寻找具有抗癌活...     

含硅芳香二胺的合成及其聚酰亚胺硅氧烷的热性能

从ｐ－或ｍ－氯苯胺出发，经三步反应合咸位置弄构的四甲基［双（苯胺）］二硅氧烷和六甲基［双（苯胺）］三硅二氧烷，总产率为２５％．与芳香二胺和芳香四酸二酐共聚得聚酰亚胶硅氧烷．研究了共聚物在玻璃化转变区的热松弛行为．对位异构体的共聚物，其分子链段的构象熵大，运动较易．     

对硝基二苯胺的一个新制法

对硝基二苯胺的一个新制法韦长梅，周建峰（淮阴师范专科学校化学系，江苏省２２３００１）对硝基二苯胺（ｐ－Ｎｉｔｒｏｄｉｐｈｅｎｙｌａｍｉｎｅ）是重要的有机试剂和合成中间体，可用作橡胶稳定剂和染料中间体［１］、合成抗乙酰胆碱能的抑制剂和溃疡抑制剂［２］。...     

Ag/ZIF-90自组装薄膜的制备及SERS活性研究

合成了金属有机框架化合物沸石咪唑框架-90(ZIF-90)溶胶和ZIF-90晶体薄膜,分别以这2种材料为基底,制备出了Ag@ZIF-90复合材料和Ag/ZIF-90自组装薄膜.通过傅里叶变换红外(FT-IR),X射线衍射(XRD),扫描电子显微镜(SEM)对产物进行表征,分析了它们的形貌和结构特征.以罗丹明6G(R 6G)作为检测分子,对所制备材料的表面增强拉曼散射(SERS)性能进行测试.结果表明制备出的Ag/ZIF-90自组装薄膜具有好的SERS性能,而ZIF-90本身的拉曼峰并不会对Ag/ZIF-90自组装薄膜的SERS检测效果产生影响.这种材料可以作为一种较好的表面增强拉曼(SERS)活性基底,在农药残留检测方面具有很好的应用前景.     

对DEPT实验技术的一点改进

将DEPT -1 3 5实验的 1 3 5° -脉冲分成一个 90°脉冲和一个 4 5°脉冲 ,通过相位循环 ,设计了两个新的DEPT实验分别称为DEPT-90 -4 5和DEPT -90 +4 5。DEPT -90 -4 5谱中只有 -CH3的吸收峰。DEPT -90 +4 5谱中没有 >CH -的吸收峰 ,其 -CH3为正信号 ,-CH2 -为负信号。实验结果显示 ,对比DEPT -90谱 ,这两个新的DEPT谱中完全没有所选基团之外的残余干扰信号 ,而且DEPT -90 -4 5谱比DEPT-90 +4 5谱更好。     

Ag/ZIF-90自组装薄膜的制备及SERS活性研究

合成了金属有机框架化合物沸石咪唑框架-90(ZIF-90)溶胶和ZIF-90晶体薄膜,分别以这2种材料为基底,制备出了Ag@ZIF-90复合材料和Ag/ZIF-90自组装薄膜。通过傅里叶变换红外(FT-IR),X射线衍射(XRD),扫描电子显微镜(SEM)对产物进行表征,分析了它们的形貌和结构特征。以罗丹明6G(R 6G)作为检测分子,对所制备材料的表面增强拉曼散射(SERS)性能进行测试。结果表明制备出的Ag/ZIF-90自组装薄膜具有好的SERS性能,而ZIF-90本身的拉曼峰并不会对Ag/ZIF-90自组装薄膜对目标分子的SERS检测效果产生影响。这种材料可以作为一种良好的SERS检测基底,在农药残留检测方面具有很好的应用前景。     

Structure-Based Design,Synthesis, and Biological Evaluation of Hsp90β-Selective Inhibitors

The 90 kDa heat shock proteins (Hsp90) are molecular chaperones that are responsible for the folding and/or trafficking of ∼400 client proteins, many of which are directly associated with cancer progression. Consequently, inhibition of Hsp90 can exhibit similar activity as combination therapy as multiple signaling nodes can be targeted simultaneously. In fact, seventeen small-molecule inhibitors that bind the Hsp90 N-terminus entered clinical trials for the treatment of cancer, all of which exhibited pan-inhibitory activity against all four Hsp90 isoforms. Unfortunately, most demonstrated undesired effects alongside induction of the pro-survival heat shock response. As a result, isoform-selective inhibitors have been sought to overcome these detriments. Described herein is a structure-based approach to design Hsp90β-selective inhibitors along with preliminary SAR. In the end, compound 5 was shown to manifest ∼370-fold selectivity for Hsp90β versus Hsp90α, and induced the degradation of select Hsp90β-dependent clients. These data support the development of Hsp90β-selective inhibitors as a new paradigm to overcome the detriments associated with pan-inhibition of Hsp90.     

Six IPR isomers of C90 fullerene captured as chlorides: carbon cage connectivities and chlorination patterns

Three C(90) fractions were isolated by multi-step HPLC from fullerene soot obtained from direct current (DC) arc discharge of undoped graphite rods. C(90) of each fraction was chlorinated with VCl(4) or SbCl(5) in ampoules at 290-310 °C, affording a series of C(90)Cl(n) compounds. Single-crystal X-ray crystallography with the use of synchrotron radiation resulted in structure elucidation of seven C(90)Cl(n) compounds containing six different isolated pentagon rule (IPR) C(90) cages (the number of the C(90) isomer is given in the parentheses): C(90)(46)Cl(32) (I), C(90)(34)Cl(32) (II), C(90)(35)Cl(24) (III), and C(90)(35)Cl(28) (IV), C(90)(32)Cl(24) (V as co-crystals with III), co-crystals of C(90)(30)Cl(22) and C(90)(28)Cl(24) (VI), and C(90)(28)Cl(24) (VII). Cage connectivities of C(90) isomers 35 and 28 have been crystallographically confirmed for the first time. The chlorination patterns of the C(90)Cl(n) molecules are discussed in terms of the formation of isolated aromatic systems and isolated C=C double bonds on the fullerene cage. The distribution of six C(90) isomers in three HPLC fractions is compared with data from the literature.     

Progress in Molecular Chaperone Regulation of Heat Shock Protein 90 and Cancer

Heat shock protein 90 (HSP90) is a member of genetically conserved heat shock protein family. As an important molecular chaperone in eukaryotic cells, HSP90 plays a key regulatory role in maintaining cellular protein homeostasis. HSP90 clients encompass a wide range of proteins, thus HSP90 is involved in diverse biological process. With the deeper study, it is found that HSP90 takes an important part in the development and metastasis of cancer, and has become a promising target for the study of anticancer biology. In this review, the progress of HSP90 as molecular chaperone and its relationship with cancer are discussed.     

Reinventing Hsp90 Inhibitors: Blocking C‐Terminal Binding Events to Hsp90 by Using Dimerized Inhibitors

Heat shock protein 90 (Hsp90) is a molecular chaperone (90 kDa) that functions as a dimer. This protein facilitates the folding, assembly, and stabilization of more than 400 proteins that are responsible for cancer development and progression. Inhibiting Hsp90’s function will shut down multiple cancer‐driven pathways simultaneously because oncogenic clients rely heavily on Hsp90, which makes this chaperone a promising anticancer target. Classical inhibitors that block the binding of adenine triphosphate (ATP) to the N‐terminus of Hsp90 are highly toxic to cells and trigger a resistance mechanism within cells. This resistance mechanism comprises a large increase in prosurvival proteins, namely, heat shock protein 70 (Hsp70), heat shock protein 27 (Hsp27), and heat shock factor 1 (HSF‐1). Molecules that modulate the C‐terminus of Hsp90 are effective at inducing cancer‐cell death without activating the resistance mechanism. Herein, we describe the design, synthesis, and biological binding affinity for a series of dimerized C‐terminal Hsp90 modulators. We show that dimers of these C‐terminal modulators synergistically inhibit Hsp90 relative to monomers.     

Development of a Grp94 inhibitor

Heat shock protein 90 (Hsp90) represents a promising therapeutic target for the treatment of cancer and other diseases. Unfortunately, results from clinical trials have been disappointing as off-target effects and toxicities have been observed. These detriments may be a consequence of pan-Hsp90 inhibition, as all clinically evaluated Hsp90 inhibitors simultaneously disrupt all four human Hsp90 isoforms. Using a structure-based approach, we designed an inhibitor of Grp94, the ER-resident Hsp90. The effect manifested by compound 2 on several Grp94 and Hsp90α/β (cytosolic isoforms) clients were investigated. Compound 2 prevented intracellular trafficking of the Toll receptor, inhibited the secretion of IGF-II, affected the conformation of Grp94, and suppressed Drosophila larval growth, all Grp94-dependent processes. In contrast, compound 2 had no effect on cell viability or cytosolic Hsp90α/β client proteins at similar concentrations. The design, synthesis, and evaluation of 2 are described herein.     

Separation of yttrium-90 from strontium-90 via colloid formation

No-carrier-added ⁹⁰Y was separated from ⁹⁰Sr via colloid formation of ⁹⁰Y in basic media. The mixture was passed through glass wool or membrane filter. The filtrate contained ⁹⁰Sr, while ⁹⁰Y was retained on glass wool/membrane filter. Yttrium-90 was extracted with 0.1 M HCl. Contamination of ⁹⁰Sr was <0.0001%. More than 98% labeling yield of ⁹⁰Y-EDTMP was confirmed by paper chromatography.     

Separation of yttrium from strontium in the aqueous phase of the water/nitrobenzene system

A rapid separation of carrier-free ⁹⁰Y in the aqueous phase of the water/nitrobenzene extraction system from an ⁹⁰Y/⁹⁰Sr generator is proposed. After a three-stage extraction, the chemical yield of ⁹⁰Y in the final aqueous phase was almost 90%, while the ⁹⁰Sr radionuclide impurity in this phase containing carrier-free ⁹⁰Y was about 10^–10%.