Synthesis and Crystal Structure of 9-（ 4-M e tho xylphen yl ）-1,8-dioxo-3,4,5,6,7,9hexahydroxanthene under Microwave Irradiation

1INTRODUCTIONInthepastfewyears,potassiumchannelacti-vatorshavegainedincreasingattentionbecauseoftheirclinicalpotentialapplicationsinvariousdiseases.Oneofthemostpotentcompoundsamongthisnewclassofdrugsisthebenzopyranderivativecroma-kalim[1～4].Benzopyranaswellasitsderivativesex-hibitsextensivepharmacologicalandbiologicalacti-vities[5],suchasantibacterialactivities[6,,antitumor7]activity[8],hypotensiveeffect[9],antiproliferationef-fect[10],etc.Thetitlecompoundbearingabenzo-pyranstructuraluni…     

Disposable ionic liquid coating for headspace solid-phase microextraction of benzene, toluene, ethylbenzene, and xylenes in paints followed by gas chromatography-flame ionization detection

Solid-phase microextraction (SPME) with a disposable ionic liquid (IL) coating was developed for headspace extraction of benzene, toluene, ethylbenzene, and xylenes (BTEX) in paints. The SPME fiber was coated with IL prior to every extraction, then the analytes were extracted and desorbed on the injection port of gas chromatography, and finally the IL coating on the fiber was washed out with solvents. The coating and washing out of IL from the fiber can be finished in a few minutes. This disposable IL-coated fiber was applied to determine BTEX in water-soluble paints with results in good agreement with that obtained by using commercially available SPME fibers. For all the four studied paints samples, the benzene contents were under the detection limits, but relatively high contents of toluene, ethylbenzene and xylenes (56-271 microg g(-1)) were detected with spiked recoveries in the range of 70-114%. Compared to the widely used commercially available SPME fibers, this proposed disposable IL-coated fiber has much lower cost per determination, comparable reproducibility (RSD < 11%), and no carryover between each determination. Considering that IL possess good extractability for various organic compounds and metals ions, and that task-specific IL can be designed and synthesized for selective extraction of target analytes, this disposable IL coating SPME might has great potential in sample preparation.     

杯芳烃的分子设计(Ⅵ)--一种新的杯[4]磺胺衍生物的合成及晶体结构

杯芳烃是由酚单体通过亚甲基在羟基邻位桥连而成的环状低聚物, 它具有可调的杯状疏水空腔, 结构柔性较大, 构象可变, 并对中性分子和有机、无机离子具有选择性配位能力. 因此, 在其上下缘进行化学修饰所得到的杯芳烃衍生物可广泛应用于萃取分离、离子选择性电极、色谱分析、功能材料、催化及模拟酶等研究领域[1～4].     

Pd_2(dba)_3/BINAP催化合成1,4-双-(4′-苯胺基苯酰基)苯

以Pd2(dba)3/BINAP催化1,4-双-(4′-溴苯酰基)苯和苯胺反应,合成了1,4-双-(4′-苯胺基苯酰基)苯,其结构经UV,1HNMR,13CNMR和元素分析表征。     

催化裂化汽油脱硫添加剂USY/ZnO/Al2O3的性能评价

 在固定流化床催化裂化装置上，以减压蜡油为原料，对制备的U\r\nSY／ZnO／Al2O3催化裂化汽油脱硫添加剂的性能进行了评价．结果表明\r\n，随着添加剂添加量和剂油比的增加，生成汽油的硫含量降低．在500\r\n℃和剂油比为5的条件下，在FCC平衡催化剂中添加30％的添加剂时，汽\r\n油的硫含量可由不加添加剂时的1230μg／g降低到770μg／g左右．添\r\n加剂的添加量（10％）较低时，对催化裂化产物的分布基本没有影响；\r\n添加30％的添加剂时，焦炭的产率有所增加，但汽油收率基本不变．X\r\nRD表征结果表明，USY／ZnO／Al2O3添加剂中的ZnO对USY的晶相结构有\r\n一定的破坏作用，但随着反应与再生次数的增多，ZnO与Al2O3之间形成\r\n较为稳定的锌铝尖晶石结构，使添加剂的性能趋于稳定．     

微波辅助合成发光可调ZnS∶Cu纳米晶

以巯基丙酸(MPA)为稳定剂, 利用微波辐射加热方法制备了水溶性的Cu掺杂的ZnS纳米晶. 通过改变微波条件, 可以在460～572 nm之间实现对ZnS∶Cu纳米晶发射峰位的连续调控. 通过XRD、 UV-Vis、荧光及荧光衰减对ZnS∶Cu纳米晶的结构和发光性质进行了详细探索, 并利用时间分辨荧光光谱对其发光机理进行了初步研究.     

Crystal Structure, Infrared Spectrum and Isotope Effect of Uranium-Crown Ether Complexes

According to the experiment results of X-ray diffraction and IR, the reduced partition function ratio (RPFR) and the contribution of various related vibration modes of uranium-crown ether complex (DCH18C6·H_3O)_2UO_2Cl_4 were theoreticallv calculated in detail. The equilibrium constant K_(eq) (that is, the single stage isotopic separation factor α) of exchange reaction for uranium isotopic chemical exchange system UO_2~(2+)(H_2O)_5—(DCH18C6.H_3O)_2UO_2Cl_4 is estimated to be 1.000746 at 12℃ and 1.000672 at 29℃, respectively, which are quite close to the experimental values 1.0010±0.0002 arid 1.0012±0.0004. Theoretical analysis shows that in the course of forming the complex of uranium with crown ether, the coordinated water of uranium is stripped, which performs a key action on the remarkable isotope effect for this system.     

二碘化钐促进的二硫代氨基甲酸酯和硫代氨基甲酸酯的还原断裂反应

室温下SmI2-THF-HMPA-t-BuOH体系可顺利地将二硫代氨基甲酸酯还原断裂得到二硫醚和硫代甲酰胺; 同样条件下, 硫代氨基甲酸酯还原断裂得到二硫醚篅34The reductive cleavage of dithiocarbamic esters are promoted by the SmI2-HMPA-THF-t-BuOH System successfully to give disulfides and thiocarboxamides at room temperature in good yields; The reduction of thiocarbamic esters are also promoted by the same system to give disulfides and carboxamides.     

Photo-induced Charge Separation of p-Tricyanovinyl-N,N-Dialkylanilines

In this paper,p-tricyanovinyl-N,N-dialkylanilines were synthesized as model compounds and through their spectroscopic behavior,the photo-induced electron transfer,charge separation were discussed and the aggregation in DMSO-H_2O system was investigated.     

丙烯酸甲酯-氰尿酸三烯丙酯共聚物的合成及其孔结构的研究Ⅰ.

氰尿酸三烯丙酯(TAC)与丙烯酸甲酯(MA)在致孔剂如环己烷、正丁醚或甲苯-汽油(200~#)存在下,用悬浮聚合得到一系列大孔共聚物。对这些共聚物孔结构的研究表明,它们的平均孔径达10000—80000(?),同时研完了致孔剂的分子结构和用量对共聚物孔结构的影响,并初步讨论特大孔共聚物形成的机理。