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The influence of microwave radiation on Ullmann reaction has been investigated by three Ullmann reactions, including triphenylamine formed by treating the diphenylamine with bromobenzene or Chlorobenzene which substitutes Iodobenzene; 4,4\'-dimethyltriphenylamine formed by treating 4,4\'-dimethyldiphenylamine with bromobenzene which substitutes Iodobenzene; 4,4\',4-trinitrotriphenylamine formed by treating 4-chloronitrobenzene with p-nitroaniline in this paper.

实验表明,在微波辐射条件下,顺式比反式迈克尔反应活性高;若在丁烯二酸的双键上引入甲基后,降低了进行迈克尔加成反应的活性;引入酯基对双键的影响比腈基有利于进行迈克尔反应,丙烯酸甲酯较丙烯腈的迈克尔反应活性高。

The optimal measuring conditions were investigated. The results indicated that the catalytic reaction to Pt and bromocresol purple was the first-order reaction. The apparent activation energy was 217.4kJ/mol and the maximum absorption wavelength of fading reaction was at 434 nm. The linear range of Pt was 0.16-4.0μg/L and the detection limit was 2.5×10^(-11)g/mL. Most of common ions had no interference with the determination, while ten multiples of Ru, Rh and Os had interference with the determination of Pt. Therefore.

选择了最佳测定条件,实验结果表明,催化反应对铂和溴甲酚紫为一级反应,反应的表观活化能为217.4kJ/mol,褪色反应的最大吸收波长为434nm,方法测定R哪的线性范围为0.16~4.0μg/L,检出限为2.5×10^(-11)g/mL,大多数常见离子不干扰测定,10倍以上的Ru,Rh和Os对测定有干扰,可在测定前分离除去。

Butadiene was polymerized to some extent in the presence of binary catalyst system NdCl33iPrOHAlEt3 in toluene and the allylchloride was then added to the solution in order to cyclize the formed polybutadiene and cyclopolymerize the unreacted butadiene monomers.

采用NdCl3·3i-PrOH-AlEt3稀土催化剂进行丁二烯的顺式聚合,在聚合过程中引入烯丙基氯,进行分子内环化反应以及单体的环聚反应。考察了稀土催化剂用量、n/n(AlEt3)、环化时间、反应温度、单体浓度等对环化反应的影响,并对产物进行了红外光谱、核磁共振光谱的表

A novel one-step green process for synthesis of glutaric acid by selective oxidation of cyclopentene was investigated.

研究了以环戊烯为原料、草酸为有机络合剂、H2O2为氧化剂,在催化剂钨酸(H2WO4)的作用下一步合成戊二酸的绿色新过程,考察了氧化剂的含量、反应物配比、催化剂用量、反应温度、反应时间等对反应的影响。

The UV and IR spectroscopic studies of the monomer films showed that the photoreaction ratio of monomer (about 50%) was higher than the corresponding photosensitive polymer (about 10%, PVCi). The polarized IR spectra proved that obvious anisotropic absorption was displayed in the irradiated photosensitive film. With polarizing microscopy method, we found that these kinds of photoalignment films exhibited good alignment ability, and the stability of the photoalignment film could reach about 100℃. 2 A photosensitive self-assembled monolayer was fabricated that contained photo-cycloadditable groups, such as, coumarin and cinnamate. The reaction process were detected by contact angle method because the IR absorption of monolayer was very weak. The photosensitive self-assembled monolayer promote uniform alignment of nematic liquid crystals by LPUV, and it thermal stability could reach about 130℃. 3 A cationic bolaform amphiphiles was synthesized that had two photosensitive double bonds, and can be polymerized by ultraviolet. A layer-by-layer self-assembled deposition film was prepared in aqueous solution by using this material and poly (sodium 4-styrenesulfonate). The UV-Vis. spectra proved that the multilayers film was uniform and layer-by-layer. When LPUV irradiated the film, the photopolymerizable double bond underwent [2+2] cycloaddition, and the production of the reaction distributed along the polarized direction of incident LPUV. Polarized UV-Vis. spectra indicated that the irradiated self-assembled multiplayer film was anisotropic, and the dichromic ration is about 0.09, it is higher than the spin-coating method of photosensitive polymer or monomer. We used this anisotropic film as alignment layer of nematic liquid crystals, and obtained a uniform and stability alignment result, the static contrast ratio is about 100, which is very close to application of liquid crystal device. This thesis is an instance that the photochemical material was used in the physics region of liquid crystals, the route that was from photosensitive monomer, self-assembled monolayer film to self-assembled multiplayer film was undergone, by this logical research method photoailgnment of liquid crystal was extended and consummated.

围绕上述思路开展了如下工作:1合成了三种可进行光二聚反应的光敏小分子单体,LPUV 辐照制作了光控取向膜;用紫外-可见光谱法和红外光谱法分析了薄膜中的光化学反应,发现小分子的光反应程度可达到50%以上,至少比光敏高分子高出5倍;薄膜的偏振红外光谱证实,经过LPUV 辐照后薄膜出现了明显的各向异性;将小分子光控取向膜制成液晶器件,在偏光显微镜下观察看到均匀一致的液晶取向;并且热稳定性达到100℃左右,接近实用化要求。2制备了含肉桂酸、香豆素基团的自组装单层膜;采用接触角的方法监测自组装反应的动力学过程;紫外-可见光谱证实了自组装单层膜在石英基板表面形成;自组装单层膜经LPUV 辐照后能诱导液晶均匀取向,而且热稳定性可达130℃,热稳定性进一步提高。3合成了含有光敏双键的双季铵盐,在水溶液状态下将它和聚乙烯基苯磺酸钠沉积生成layer-by-layer 自组装多层膜,紫外-可见光谱证实这是一个逐层均匀的沉积;在LPUV 照射下,自组装膜中的光敏双键按照偏振方向发生[2+2]环加成反应,形成取向膜,用二向色性值评价的分子取向度高于高分子及小分子光控取向膜的水平;实验证明用自组装多层膜制成的液晶器件亮暗态均匀,静态对比度约为100,达到实用化器件的水平。

The thermoinduced coloration system of fluorane/iodonium salt has been investigated. The kinatic studies of thermoinduced color development reaction in polymer film was performed. It was found that two different phenomena appeared in the relationship between reaction rate constant and temperature. A very low value of k〓(0〓mol〓·l·s〓) and very high energy of activation E〓(149 KJ·mol〓) observed in the region of low temperature, whereas a larger value of k〓(1~10 mol〓·1·s〓) and smaller energy of activation (E〓33 KJ·mol〓) displayed in the region of high temperature of 150℃.

研究了荧烷/碘鎓盐热致显色反应体系,进行了分子膜中热生色反应动力学的研究,发现热生色速度常数k〓和温度关系呈现二种不同情况:在低温区,k〓值很小(<10〓mol·1·s),活化能很大(E〓=149KJ·mol〓);而在高温区,k〓值较大(1~10〓mol·1·s),活化能较低(E〓=33KJ·mol〓),它们的转折点位于温度(T〓=119℃),表明高于T〓是进行热致显色反应的重要条件;考虑到它们用作热记录介质的可能,研究了熔融状态中热生色反应。

As to MNa-ZSM-5, the order is CuNa-ZSM-5〓AgNa-ZSM-5>CeNa-ZSM-5> CoNa-ZSM-5〓FeNa-ZSM-5>Na-ZSM-5. Among the samples tested, CoHZSM-5 shows the highest activity, the conversion of NO is about 60%, and the activity is higher than that of CoNa-ZSM-5 with the same exchanged level. Suggests that the exist of some Bronsted acidity is benefited for this reaction. For Fe-ZSM-5, the activity are changed obviously with the various of preparation condition. It was also found that mordenite zeolite is a good support for this reaction.

其中,Co-HZSM-5表现出最佳的反应活性,NO的最高转化率达60%以上,并且活性明显高于具有相同交换度的CoNa-ZSM-5,表明适量的酸中心存在有利于该反应的进行;对于Fe-ZSM-5,制备条件不同Fe-ZSM-5的反应活性影响很大,反应的活性中心应是处在交换位上的铁离子;另外,通过考察不同载体对铁离子交换分子筛催化剂反应性能的影响,发现丝光分子筛也是较好的催化剂载体。

Mixed chlorotoluenes photo-chlorination experiments in a loop reactor were made, the effects of chlorine flow, temperature and p-/o- chlorotoluene initial ratio on mixed chlorotoluenes photo-chlorination were researched. The relations between the concentration of each component and time under different conditions were measured. The rule and the suitable process parameters of the photochlorination of p-chloromethyl benzene in the side chain were obtained.

本文在环流反应器中进行了邻、对氯甲苯混合光氯化反应试验,分别考察了不同氯气流量、不同氯化温度和不同对/邻氯甲苯初始配比对对、邻氯甲苯侧链光氯化反应的影响,实测了反应液中各组分浓度随时间的变化关系,得出了对、邻氯甲苯的侧链光氯化反应规律和适宜的工艺条件。

Seven of them have not been reported.Their structures were confirmed by IR,~1HNMR,MS,and element analysis. 4.Meanwhile,the green methylation procedure of imides was developed by using dimethyl carbonate as methylation reagent.A series of imides,for example,phthalimide,3,4-dibromo-maleimide and succincide were used for substrates.The effects of DABCO(1,4-diazabicyclo [2.2.2]octane)and DBU(1,8-diazabicyclo[5.4.0]undec-7-ene)as a catalyst in this kind of reactions were investigated.2-Bromo-3-(1-methylindolyl-3-yl)-1-methyl-1H-pyrrole-2,5-dione was prepared by using dimethyl carbonate,which further expanded the use of dimethyl carbonate,as a green agent in organic synthesis.

在以硫酸二甲酯为甲基化试剂对3,4-二溴马来酰亚胺进行N-甲基化反应合成3,4-二溴-N-甲基马来酰亚胺的同时,以碳酸二甲酯为甲基化试剂,对3,4-二溴马来酰亚胺、邻苯二甲酰亚胺、琥珀酰亚胺等酰亚胺类化合物的N-甲基化反应进行了研究;考察了1,4-二氮杂双环[2.2.2]辛烷,1,8-二氮杂双环[5.4.0]十一碳-7-烯、碳酸钾和四丁基溴化铵等作为催化剂对碳酸二甲酯N-甲基化反应的反应时间和收率等的影响,并应用碳酸二甲酯为甲基化试剂,合成了N-甲基-3-溴-4-(1-甲基-吲哚-3)-马来酰亚胺。

The plant and environment interactions and the molecule mechanism, include light acceptors and its message transductions, heat shock and its protein induced, phytopathological defensive reaction and its elicitors and related proteins, mechanical injury message and the signal introduction.

环境刺激及其反应的分子机制:光受体及其信号转导;热激及热激蛋白、功能与热激反应的信号转导;植物的病理防御反应,激发子及其结合蛋白与防御反应的信号转导;机械与伤害信号分子及其信号转导。

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As she looked at Warrington's manly face, and dark, melancholy eyes, she had settled in her mind that he must have been the victim of an unhappy attachment.

每逢看到沃林顿那刚毅的脸,那乌黑、忧郁的眼睛,她便会相信,他一定作过不幸的爱情的受害者。

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