Synthesis,Crystal Structure,and Biological Activity of 4-Chlorobenzaldehyde (2-trifluoromethylTrifluoromethyl-5,6,7,8-tetrahydrobenzo[4 ,5]-thieno[2,3-d]pyrimidin-4-yl)hydrazone Monohydrate

The novel title compound 4-chlorobenzaldehyde (2-trifluoromethyl-5,6,7,8- tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4-yl)hydrazone monohydrate (C18H14ClF3N4SH2O, Mr = 428.86) has been synthesized by a condensation reaction of 4-chlorobenzaldehyde with (2-trifluoromethyl-5,6,7,8-tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4-yl)hydrazine, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 7.4252(7), b = 26.344(2), c = 10.3095(9) , = 109.407(2)°, V = 1902.0(3) 3 , Z = 4, Dc = 1.498 g/cm3 , μ = 0.356 mm-1 , F(000) = 880, the final R = 0.0564 and wR = 0.1681 for 2343 observed reflections with I > 2 (I). X-ray diffraction analysis reveals that the title hydrazone molecule is nearly planar except for the cyclohexene and trifluoromethyl moieties. In the crystal packing, the molecules form stacks by a three-dimensional framework, which results from intermolecular N(3)-H(3)···O(1), O(1)-H(1B)···N(2), O(1)- H(1B)···N(4) and O(1)-H(1A)···F(1) hydrogen bonds via water molecules together with π-π stacking interactions. Molecular geometry of the title compound in the ground state optimized by B3LYP functional with 6-311G** basis sets indicates that the calculations are in agreement with the experimental data. The preliminary bioassay suggested that the title compound exhibits relatively good fungicidal activity against Fusarium oxysporium f.sp.vasinfectum and Dothiorella gregaria.     

含1,3,4-噻二唑环吡唑并[3,4-d]嘧啶类化合物的合成及生物活性

通过5-氨基-4-氰基-1-苯基吡唑与甲酸发生环合、再经氯化和芳香族亲核取代反应,合成了12种新的含1,3,4-噻二唑环吡唑并[3,4-d]嘧啶类化合物.目标化合物的结构经红外光谱、核磁共振氢谱、质谱和元素分析方法予以确认.初步的生物活性测定试验表明,在50 mg/L浓度下,大部分目标化合物对小麦纹枯病菌(Rhizoctonia cerealis)表现出较好的杀菌活性,其中化合物5b,5d和5j的抑菌率超过90%.     

MoO3—SiO2表面复合物金属催化剂载体的制备与表征

采用ＭｏＯＣｌ４的盐酸溶液负载于ＳｉＯ２的表面反应法，制备了负载型和键联型两种ＭｏＯ３－ＳｉＯ２（ＭｏＳＯ）表面复合物载体。利用红外光谱法研究了ＭｏＳＯ的表面构造及其化学吸附性能；并利用ＴＰＲ技术考察了该表面复合物载体对负载金属Ｐｄ，Ｃｕ氧化物还原过程的影响。     

铝材表面状态对TiO2薄膜光催化性能和光致亲水性的影响

在纯铝片和具有氧化铝层的铝片上用提拉法制备TiO2/Al和TiO2/Al2O3/Al样片,通过FTIRATR技术和密闭间歇式反应装置分别考察了TiO2薄膜对油酸和乙烯的光催化降解性能,通过测试接触角考察TiO2薄膜的光致亲水性.结果表明,TiO2/Al2O3/Al对油酸的光降解性能比TiO2/Al的好,但其光催化氧化乙烯性能和光致亲水性能较差.这种差别可通过不同过程的作用机理和Al与TiO2表面的电子转移作用得到较好解释,由此得出TiO2薄膜的光催化性能与光致亲水性可能是两种既有联系又相互独立的性质     

TiO2胶粒在铝合金表面的电泳沉积及所制薄膜的光催化性能研究

TiO₂ membranes were prepared on aluminum-alloy thin plates by electrophoretic deposition and dip coating in a colloid solution of TiO₂, respectively. The photocatalytic activity of TiO₂ membrane was compared using ethylene as reactant, and the crystal and morphological structure of the membrane were characterized by XRD and SEM. The results showed that a more compact membrane with high loading of TiO₂ but lower photocatalytic activity of unit TiO₂ mass was obtained by electrophoresis compared with dip coating method. The addition of polyethylene glycol (PEG) to the sol of TiO₂ could improve the specific photocatalytic activity (ethylene conversion per unit mass TiO₂ and unit area of membrane piece) of the electrophoresis-membrane prepared from the sol, but could not change the specific photocatalytic activity of the dip-coating membrane from the sol. The ethylene conversion on the electrophoresis membrane prepared from the sol containing PEG (50 g·L^-1) was 9 times of that on the dip coating membrane. The effect of PEG on the properties of electrophoresis-membrane of TiO₂ was attributed to the change of electrokinetic properties of sol. Addition of PEG decreased ζ potential value of the sol and the mobility of the sol particle, increased viscidity of the colloid, thus decreasing both the electrophoresis deposition velocity of colloid particles and the electroosmosis velocity of diffuse layer of colloid particles. These favored the formation of a low compact and porous membrane on the electrode in electric field, and thus increasing the availability of TiO₂ in photocatalytic process.     

基于三蝶烯结构D3h对称性聚酰亚胺的合成及性能研究

以四氯邻氨基苯甲酸和蒽经Diels-Alder反应得到1,2,3,4-四氯三蝶烯,再经硝化、还原得到2,6-二氨基-13,14,15,16-四氯三蝶烯二胺单体.该二胺与双酚A二酐(BPADA)、六氟二酐(6FDA)和3,3’,4,4’-二苯甲酮四羧酸二酐(BTDA)经两步法缩聚得到系列聚酰亚胺.对2,6-二氨基-13,14,15,16-四氯三蝶烯二胺单体进行了1H-NMR,13C-NMR,FTIR表征,对所合成聚酰亚胺进行了1H-NMR、FTIR结构表征及溶解性、热性能、特性粘度、BET等测试.结果表明,含四氯三蝶烯结构的聚酰亚胺具有优异的溶解性,能溶于DMAc、DMF、NMP、THF、吡啶、间甲酚等有机溶剂,其中基于双酚A二酐和六氟二酐的聚酰亚胺在室温下能溶于氯仿中.聚合物具有良好的热性能,在0~300℃之间没有发现其玻璃化转变温度以及10%的热失重温度均高于500℃.聚合物可形成颜色较浅的透明薄膜,其中基于双酚A二酐的聚酰亚胺薄膜为无色透明.基于六氟二酐的聚酰亚胺BET比表面积为370 m2/g,是一种新型多孔聚合物.     

铝片表面阳极氧化铝膜的光催化作用

采用阳极电化学氧化在铝片表面制备出表面含有氧化铝膜的铝片(AAO/Al), 分别用FTIR-ATR技术和密闭间歇式反应装置考察了该样片对油酸和乙烯的光解作用, 结合UV-DRS和FTIR表征结果对薄膜在油酸和乙烯光解中的作用进行了探讨. 结果表明：AAO/Al能够吸收小于265 nm的紫外光, 而无AAO膜的铝片对波长大于220 nm的紫外光没有任何吸收；254 nm紫外光照射下AAO/Al对油酸和乙烯的光解具有明显的促进作用, 光照3 h油酸的分解率达到70%, 乙烯也有9%的分解, 但相同条件下在无AAO膜的铝片上, 油酸的光解率仅为30%, 乙烯几乎不分解；然而, 在365 nm紫外光照射下, AAO/Al同纯铝片一样对两反应物的光解都没有任何促进作用. 分析认为, AAO膜能吸收254 nm的紫外光和对有机物分解具有光催化作用的可能原因是在AAO膜结构中存在过量的Al原子和氧空位.     

Mg-Al 类水滑石/二氧化钛异质复合纳米晶光催化氧化苯的性能

 采用过饱和沉淀法合成 n(Mg)/n(Al) = 2 的 Mg-Al 类水滑石化合物 (Mg-Al-HT), 再用水热法将它与钛胶复合, 制得 Mg-Al-HT/TiO2 异质复合光催化剂. 采用 X 射线粉末衍射、透射电子显微镜、场发射扫描电子显微镜、低温 N2 吸附-脱附、紫外-可见漫反射光谱和热重等技术对催化剂结构、成分和性质进行了表征. 结果表明, 在波长 365 nm 的紫外光照射降解苯的反应中, Mg-Al-HT/TiO2 异质复合光催化剂表现出优于单一的 TiO2 或 Mg-Al-HT 催化剂的光催化活性, 且稳定性更高; 同时讨论了该复合催化剂性能优异的原因. 另外, 运用电子顺磁共振技术检测到体系中存在羟基自由基等活性物种, 并据此提出了 Mg-Al-HT/TiO2 异质复合纳米晶催化剂光催化降解苯的反应机理.     

紫菀中的一个新寡肽

紫菀肽C为白色粉末,m.p.250～252℃,[α]_D—4.9°(c=0.33),对Ninhydrin反应呈阴性,Ehrlich反应呈阳性。IRυ_(max)~(KBr)(cm~(-1))示有羟基(3304)、酯羰基(1749)和酰胺键(1651)。UV(nm):208(1.39×10~4,MeOH),267(1.82×10~4)。以上结果表明为一个肽类化合物。将该化合物用6mol/L盐酸水解,用氨基酸分析仪检测出丝氨酸(Ser,1mol),苏氨酸(Thr,1     

寡肽Asterin B和C溶液构象的NMR研究1: ^1H NMR归属及构象特征

Asterin B和C是从紫菀中分得的两个寡肽, 本文利用2D-NMR技术归属了它们的^1H NMR谱线, 并讨论了它们的构象特征。为进一步采用NMR和分子动力学(MD)方法研究它们的溶液构象奠定了基础。