双邻苯二酚锑二甲基羟乙铵的晶体结构

含锑配合物是治疗血吸虫病、肿瘤等的常用药物,我们曾对双邻苯二酚锑二乙基羟乙胺进行了晶体结构测定,本文简要报导双邻苯二酚锑二甲基羟乙胺的结构.锑化合物的制法与其二乙基羟乙铵衍生物类似.产物为淡黄色晶体,它在水溶液中长时间放置会变成紫黑色,因此,制得的晶体须立即用丙酮溶解进行重结晶.晶体的密度为1.667g/cm~3.按C_(16)H_(20)O_5NSb的元素分析结果(％)如下:Sb 28.3(28.5),C 43.9(44.9),N 3.3(3.3),H 4.7(4.7).括号内为理论值.     

N—BOC—8—氨甲基—2—萘甲酸的改进合成法

以２－萘甲酸为原料，经硝化，酯化，重氮化，选择性催化氢化，ＢＯＣ酸酐保护等六步反应，完成了Ｎ－ＢＯＣ－８氨甲基－２－萘甲酸（１ａ）的合成，为化合物１的合成提供了新的合成途径。     

甲烷在二元碱土金属复合体系催化剂上的氧化偶联

碱土金属氧化物或碳酸盐为多种类型甲烷氧化偶联制取C_2烃催化剂的重要组分之一.有关纯碱土金属氧化物及含氧酸盐的研究表明,这类化合物具有较强的表面碱性及高温P型半导性而对活化甲烷生成C_2烃有较高活性,关于不同碱土金属化合物之间混合形成的二元碱土金属复合体系催化剂的报导仍不多见,Aika等人曾报导用BaO与CaO或MgO混合的催化剂上在1073K时可以获得61.1%C_2烃选择性和14.2%的C_2烃收率,但BaO易在反应条件下与水反应生成Ba(OH)_2而腐蚀器壁,不利于长期操作.本文报导了一系列不同碱土金属化合物之间形成的二元碱土复合体系催化剂上甲烷氧化偶联的反应结果.结果表明,这类催化剂由于其结构稳定、活性好而值得进一步研究.     

Crystal Structure and Characterization of a Large Polyoxotungstate (NH4)21{La(H2O)5[Ni(H2O)]2As4W40O140}·53H2O

The heteropolytungstate (NH4)₂₁{La(H₂O)₅[Ni(H₂O)]₂As₄W₄₀O₁₄₀}·53H₂O is obtained by the reaction of Na₂₇[NaAs₄W₄₀O₁₄₀]· 60H₂O with NiCl₂·6H₂O, La(NO₃)₃·6H₂O and NH₄Cl at pH‐4.5. The structure and chemical composition are determined by X‐ray diffraction analysis and elemental analysis. The crystal data and main structure refinement are a = 1.9551(3) nm, b = 2.4156(4) nm, c= 3.7068(6) nm, β = 91.505(3)°, V = 17.500 (5) nm³, monoclinic crystal system with space group P2₁/n, Z = 4, R₁ = 0.0573, wR₂ = 0.0717 [I >2<s?(I)], R₁, = 0.2463 and wR₂ = 0.1199 (all data). [La(H₂O)₅] {Ni(H₂O)}₂AS₄W₄₀O₁₄₀ has C₂, symmetry. IR spectra of the ligand [NaAs₄W₄₀O₁₄₀]^27‐ and its three complexes were discussed.     

3,3,6,6-四甲基-9-邻氯苯基-1,8-二氧代-3,4,5,6,7,9-六氧化氧杂蒽的合成和晶体结构

标题化合物C23H25对O3Cl是由邻氯苯甲醛与5，5-二甲基1，3-环己二酮在N，N-二甲基甲酸腹中反应而得。结构通过单晶X-射线衍射法确定，其晶体属于单科晶系，空间群=1632。晶体结构用直接法解出，使用全矩阵最小二乘法对原子参数进行修正，最后的偏离因子为R=0．054，Rw一0．063。在晶体结构中，吡喃环与苯环之间的两面角为92．43°。     

溶液pH值对聚邻甲苯胺电化学性质的影响

本文报道了溶液pH值对聚邻甲本胺电化学性质的影响。研究结果表明,电化学合成的聚邻甲苯胺的循环伏安曲线、氧化电位、膜的颜色、充放电容量、紫外可见光谱以及氧化还原活性都受到溶液pH的影响。在低pH值的溶液中,随着扫描电位的变化,聚邻甲苯胺膜的颜色可逆地变化,而在pH4.13的溶液中进行扫描时,膜的颜色不变化,电化学活性也消失。     

Synthesis of polypiperazine-amide thin-film membrane on PPESK hollow fiber UF membrane

A new interfacial polymerization (IP) procedure is developed in order to synthesize polypiperazine-amide thin-film membrane on the inner surface of poly(phthalazinone ether sulfone ketone) (PPESK) hollow fiber ultrafiltration (UF) membrane.A hollow fiber composite membrane with good performance was prepared and studied by FT-IR and scanning electron microscopy.     

4,5-咪唑双酰腙的合成与表征

以酒石酸为原料，经成环制酸、酯化、肼解、与芳香醛缩合，制备了7个4，5－咪唑双酰腙，并用元素分析，IR，^1H NMR,^13C NMR对它们的结构进行了表征。实验结果表明，酰肼与芳香醛在冰醋酸中进行缩合酰腙化一步，具有反应快速、产率高、条件温和、操作简便等优点。     

C9‐Iridoids from Scrophularia buergeriana

Four new iridoids, buergerinins B–E ( 1 – 4 ), along with three known iridoids, were isolated from the roots of Scrophularia buergeriana. Their structures were identified on the basis of spectroscopic analysis.     

An Efficient Synthesis of Pyrazolo[3,4‐b]Pyridine Derivatives in Aqueous Media

A series of pyrazolo[3,4‐b]pyridines was synthesized by the reaction of 5‐aminopyrazole with benzylidenemalononitrile in aqueous media. The structures were characterized by IR, ¹H NMR, and elemental analysis and were further confirmed by X‐ray diffraction analysis.