（R）－2－硫代四氢噻唑－4－羧酸甲酯的合成及消旋化

Ｌ－半胱氨酸甲酯盐酸盐和二硫化碳在三乙胺存在下反应，当摩尔比为１：１．５：２时，得到的（Ｒ）－２－硫代四氢噻唑－４－羧酸甲酯，产率８０％；摩尔比为１：１．５１３．５时，得到Ｒ，Ｓ－２－硫代四氢噻唑－４－羧酸甲酯。另外，由（Ｒ）－２－硫代四氢噻唑－４－羧酸与甲醇及二氯亚硫酰反应，也得到（Ｒ）－２－硫代四氢噻唑－４－羧酸甲酯，产率为９８％，     

2—（6—甲基—2—苯并噻唑偶氮）—5—二乙氨基酚分光光度法测定微量镍

用新试剂２－（６－甲基－２苯并噻唑偶氮）－５－二乙氨基酚分光光度法测定微量镍。     

2β—氯甲基青霉烷基二苯甲酯合成方法的改进

6，6－二氢青霉烷酸二苯甲酯1β－氧化物同2β－巯基苯并噻唑反应后，与硫酰氯作用得2β－氯甲基青霉烷基二苯甲酯。     

联恶唑啉类手性配体在不对称氢迁移反应中的应用

以光学活性联恶唑啉为配体，与〔Ｉｒ（ＣＯＤ）Ｃｌ〕２（ＣＯＤ＝１，５－环辛二烯）反应，形成了４种光学活性铱络合物，考察了它们在异丙醇存在下催化苯乙酮不对称氢迁移反应的光学活性，发现４，４‘－二乙基－４，４’，５，５‘－四氢－２，２’－联恶唑啉具有较好的光学诱导效果，其光学产率最高可达３１．５％。     

改性ZSM－5分子筛催化法合成糠醇酯的研究

利用改性ＺＳＭ－５分子筛为催化剂，催化合成了丙酸糠酯，戊酸糠酯异戊酸糠酯及乙酸四氢糠酯，丙酸四氢糠酯，丁酸四氢禄酯。文中讨论了影响反应的诸因素。酯的收率为６０％～８０％之间。     

改性ZSM—5分子筛催化法合成糠醇酯的研究

利用改性ＺＳＭ－５分子筛为催化剂，催化合成了丙酸糖酯，戊酸糠酯异戊酸糖酯及乙酸四氢糖酯，丙酸四氢糠酯，丁酸四氢禄酯，文中讨论了影响反应的诸因素，酯的收率为６０％￣８０％之间。     

在三氯化铝催化下1—芳基亚胺—1—苯基丙烷与顺丁烯二酸酐的反应

１－芳基亚胺－１－苯基丙烷与顺丁烯二酸酐在三氯化铝催化下反应可得到两个产物：顺丁烯二酸单酰胺和１－芳基－５－苯基－４－甲基－２－氧代－２，５－二氢吡咯－３－乙酸。还对此反应的机理进行了探讨。     

在三氯化铝催化下1－芳基亚胺－1－苯基丙烷与顺丁烯二酸酐的反应

１－芳基亚胺－１－苯基丙烷与顺丁烯二酸酐在三氯化铝催化下反应可得到两个产物：顺丁烯二酸单酰胺和１－芳基－５－苯基－４－甲基－２－氧代－２，５－二氢吡咯－３－乙酸．还对此反应的机理进行了探讨．     

3-(2-氧代环己基)丙酸与(R)-四氢噻唑-2-硫酮-4-羧酸乙酯的反应及其量子化学研究

由L-半胱氨酸乙酯与二硫化碳在Et3N存在下反应,得到光学活性（R）－四氢噻唑－2－硫酮－4－羧酸乙酯,后者同3－（2－氧代环已基）丙酸在N,N－二环己基胺二亚胺（DCC）存在下反应,得到光学活性（R）－N－3－（2－氧代环己基）丙酰四氢噻唑2－硫酮－4－羧酯乙酯及光学活性的3－（2－氧代环己基）丙酸．用半经验的量子化学PM3方法研究反应物和产物的最优构型与电子结构．     

2—（2—氨基—4—塞唑）—（Z）—2—（叔丁氧羰甲氧亚胺基）硫代乙酸2—苯并噻唑酯 …

本文提供了一条新的合成２－（２－氨基－４－噻唑）－（Ｚ）－（叔丁氧羰甲氧亚胺）硫代乙酸２－苯并噻唑酯的工艺路线。     

N-邻羟苯基氨基酸酯亚胺化合物的合成、表征及抑菌活性

以水杨醛与氨基酸酯为原料通过Schiff碱缩合反应合成了六种水杨醛缩氨基酸酯,并采用红外、核磁对其结构进行确认表征.生物活性测试表明,N-邻羟苯基亮氨酸酯对白色念株菌的抑菌活性最强,N-邻羟苯基苯丙氨酸酯对大肠杆菌的抑菌活性最强,N-邻羟苯基甘氨酸酯对金黄色葡萄球菌的抑菌活性最强.此结果说明,氨基酸酯结构的不同是导致抑菌活性不同的根本原因.     

3-(4-氯苯基)-1,3-2H-3-苯基恶唑[3,4-a]吲哚合成

以溴化亚铜作催化剂,DMF作溶剂,用N-(o-alkynylphenyl)imines亚胺在温和条件下环合-加成反应,一步合成吲哚衍生物,结果发现恶唑类吲哚在不同催化剂、不同底物种类及反应条件下的反应速度和产率具有较大差异性.     

Diastereoselective addition of lithium enolate of γ-substituted α-diazoacetoacetate to <Emphasis Type="Italic">N</Emphasis>-sulfinyl imines

Highly diastereoselective addition of lithium enolate of γ-substituted α-diazoacetoacetate to chiral N-sulfinyl imines has been developed. The addition products were further subjected to photo-induced Wolff rearrangement or Rh(II)-catalyzed intramolecular N–H insertion to afford chiral 4,5-disubstituted 2-oxo and 3-oxo pyrrolidines, respectively.     

Stepwise radial complexation of imine groups in phenylazomethine dendrimers

Dendrimers are highly branched organic macromolecules with successive layers or 'generations' of branch units surrounding a central core. Organic-inorganic hybrid versions have also been produced, by trapping metal ions or metal clusters within the voids of the dendrimers. The unusual, tree-like topology endows these nanometre-sized macromolecules with a gradient in branch density from the interior to the exterior, which can give rise to an energy gradient that directs the transfer of charge and energy from the dendrimer periphery to its core. Here we show that tin ions, Sn(2+), complex to the imine groups of a spherical polyphenylazomethine dendrimer in a stepwise fashion. This behaviour reflects a gradient in the electron density associated with the imine groups, with complexation in a more peripheral generation proceeding only after complexation in generations closer to the core has been completed. By attaching an electron-withdrawing group to the dendrimer core, we are able to change the complexation pattern, so that the core imines are complexed last. By further extending this strategy, it should be possible to control the number and location of metal ions incorporated into dendrimer structures, which might find uses as tailored catalysts or building blocks for advanced materials.     

基于接触摩擦的多片式钢板弹簧悬架预应力的计算

采用基于接触摩擦的有限元方法,在Ansys中使用面-面接触单元建立钢板弹簧有限元模型.对一组多片式钢板弹簧悬架进行预应力的计算,并与用传统预应力计算方法得到的结果和行业推荐值进行比较分析,证明新的方法更能反映簧片实际的受力情况.由此对簧片的自由曲率半径和自由弧高进行修正,既能满足设计要求,又能提高整副钢板弹簧的使用寿命.     

利用原生质体融合技术选育高产菌株

以龟裂链霉菌(Sterpomyces rimosus)98#和76#为出发菌株,分别用溶菌酶制得2个亲本的原生质体,其中76#采用15 W紫外灯下30 cm照射25 min,100 %灭活,用PEG诱导进行了原生质体的融合.通过比较菌落外观、颜色挑选融合子328株,结合前期代谢情况进一步筛选高单位的融合菌株8株,经反复传代考察融合子的稳定性后得到1株新菌株102#,其发酵单位比亲本提高了13.0%.     

反应离子刻蚀剥层的微分霍耳法表征超浅pn结

用反应离子刻蚀(RIE)剥层的微分霍耳法(DHE)对等离子体掺杂、离子注入制备的Si超浅p n结进行了电学表征.通过对超浅p n结样品RIE剥层的DHE测试和二次离子质谱(SIMS)测试及比较,发现用反应离子刻蚀(RIE)剥层的DHE测试获得的杂质浓度分布及结深与SIMS测试结果具有良好的一致性,DHE具有良好的可控性与重复性.测试杂质浓度达1021cm-3量级的Si超浅结样品,其深度分辨率可达nm量级.     

隧道过海段水压力及渗流量计算方法

为了研究三心圆隧道复合衬砌的渗流量及不同部位水压力大小,分别利用等效面积法和等效周长法求出不同注浆圈厚度、不同注浆圈渗透系数、不同初期支护渗透系数下三心圆隧道的渗流量及不同部位水压力折减系数的解析解;并与相同条件下不同工况的数值模拟值进行对比。结果表明:计算隧道渗流量时,等效面积法得到的解与数值模拟值最大相差0. 3%;等效周长法得到的解与数值模拟值相差1. 5%。计算初期支护外水压力折减系数时,等效面积法得到的解与数值模拟值最大相差4. 8%;等效周长法得到的解与数值模拟值相差4. 6%。计算二次衬砌外水压力折减系数时,等效面积法得到的解与数值模拟值最大相差7. 6%;等效周长法得到的解与数值模拟值相差7. 8%。     

证据协力义务视野下的民事非法证据排除规则

证据协力义务的范围与强度同非法证据的数量呈反比例关系。最高人民法院《关于民事诉讼证据的若干规定》通过制度化的方式确立了民事诉讼中的非法证据排除规则。然而,司法实践中却屡屡出现对非法证据的效力作出截然相反认定的案例。非法证据排除规则在民事诉讼中的非正当性造成了上述困惑。应以证据协力义务取代民事非法证据排除规则,同时对已形成的非法证据不予排除,并追究非法取证者的刑事、民事责任。     

Supramolecular self-assembly of nickel (Ⅱ)-substituted α-Keggin-type polyoxometalate and polyaniline coated Fe2O3 hollow nanospindle for microwave absorption application

A general strategy has been developed here to supramolecular self-assembly of nickel (Ⅱ)-substituted α-Keggin-type polyoxometalate and polyaniline coated Fe₂O₃ hollow nanospindle (Fe₂O₃ hollow nanospindle@PANI/α-SiW₁₁Ni composites) via electrostatic attraction and hydrothermal method. Fe³⁺ was first hydrolyzed and polymerized into Fe₂O₃, then dissolved into [Fe(H₂PO₄)_x]^3?x, resulting in hollow structure. The polyoxometalate existed in polyaniline as a proton-doped counter-ion form, rather than as a separate crystalline state. The protons and anions entered the PANI main chain and combined with N atoms of amines and imines on the PANI chain ((-NH^?+ ?= ?)/α-[SiW₁₁Ni(H₂O)O₃₉]^6-) to form poles and bipolar delocalization into π bonds of the whole polyaniline molecular chain, which leaded to conductance and polarization. The Fe₂O₃ hollow nanospindle@PANI/α-SiW₁₁Ni composites were proven to be excellent microwave absorber in terms of reflection loss (R_L) and bandwidth. The maximum R_L value was up to ?53.6 ?dB at 3.5 ?mm and 6.9 ?GHz. The broadest absorption bandwidth exceeding ?10 dB was 6.3 ?GHz at a thickness of only 1.9 ?mm. Moreover, the ternary composites presented obvious multi-band absorption with the matching thickness range of 1.5–5 ?mm. The absorption peaks bandwidth reached as wide as 14.3 ?GHz, which included all C-Ku bands. The hollow and core-shell structures could provide non-uniform interface for the induced polarization loss and space for the reflecting and scattering of microwave. The carrier, pair-ion carrier and hydrogen bond network could lead to conduction loss. The magnetic losses were caused by eddy current effect and natural resonance. This work can lay a theoretical foundation for the design and performance regulation of new absorbing materials.