基于Willgerodt-Kindler反应的两种二茂铁羧酸的合成及机理研究

以Na2S•9H2O为催化剂, 通过Willgerodt-Kindler反应分别合成了二茂铁乙酸和1,1’-二茂铁二乙酸, 用IR, 1H NMR, MS和元素分析对产物分别进行了结构表征, 并利用GC-MS研究了该反应机理, 推测反应是由多硫阴离子进攻羰基α碳所引发, 同时讨论了影响反应的各种因素.     

3-(N-取代苯基-2-乙酰胺基)硫基-4-N-取代邻羟苯基亚胺基-5-甲基-1,2,4-三唑类化合物的合成及生物活性研究

以对称二氨基硫脲为原料,与冰醋酸反应生成5-甲基-4-氨基-1,2,4-三唑-3-硫酮(1);在弱酸性条件下,1与取代水杨醛反应生成席夫碱中间体5-甲基-4-(N-取代邻羟苯基)亚胺基-1,2,4-三唑-3-硫酮(2a～2c);最后在碱性条件下分别与N-取代苯基-2-氯乙酰胺发生烷基化反应生成15种未见报道的目标化合物3-(N-取代苯基-2-乙酰胺基)硫基-4-(N-取代邻羟苯基)亚胺基-5-甲基-1,2,4-三唑(3a～3o),其结构经IR,1H NMR,13C NMR确证.初步生物测试表明,质量分数为0.01%时,3a～3o对白色念珠菌的抑菌率均达90%以上,具有很强的抑菌活性;对金黄色葡萄球菌、大肠杆菌的抑菌率达80%以上,具有较强的抑菌活性.     

二聚体有机锡配合物{[n-Bu2Sn(O2CCH2CS2NC4H8)]2O}2的合成，表征及晶体结构(英)

The title compound, {[n-Bu₂Sn(O₂CCH₂CS₂NC₄H₈)]₂O}₂, has been synthesized by the reaction of (tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in 1∶1 molar ratio. The complex has been characterized by elemental analysis, IR and NMR. The crystal structure of it has been determined by X-ray single crystal diffraction. And the results showed that the crystal belongs to triclinic system with space group P1 and some crystal parameters: a=1.220 2(9) nm, b=1.315 8(10) nm, c=1.380 4(10) nm, α=111.215(9)°， β=99.357(9)°， γ=96.075(10)°, V=2.006(2) nm³, Z=1, F(000)=908, μ=1.489 mm^-1, D_c=1.474 g·cm^-3, R₁=0.037 5, wR₂=0.0839. The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron. Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only. CCDC: 220513.     

2,4,6-三对氨基苯氧基-1,3,5-均三嗪的合成

以三聚氯氰和对硝基苯酚为原料,经取代、还原合成了2,4,6-三对氨基苯氧基-1,3,5-均三嗪。对Pd/C水合肼、SnCl2·2H2O-HCl及Pd/C催化加氢三种不同还原体系进行比较。采用1H-NMR、FT-IR和元素分析方法对产物进行结构表征。     

Influence of nature of precursors on the formation and structure of Cu-Ni-Cr mixed oxides from layered double hydroxides

Analogous layered double hydroxides (LDHs) with the Cu²⁺/Ni²⁺/Cr³⁺ molar ratio of 1/2/1 on the brucite-like layers and interlayer anions (viz sulfate, nitrate and carbonate, respectively) were synthesized by a coprecipitation method. For the first time, the effects of interlayer anions on the structural properties of as-synthesized LDHs and resulting calcined products at 773 K were investigated by means of powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), simultaneous thermogravimetric and differential thermal analysis (TG-DTA), X-ray photoelectron spectroscopy (XPS) and temperature programmed reduction (TPR). The results indicate that the nature of interlayer anions involved within the hydrotalcite (HT)-like structure has a larger influence on the thermal stability of LDHs precursors. Calcination of well-crystallized LDHs leads to the formation of mixed metal oxides including CuO, NiO and Cu²⁺-, Ni²⁺- and Cr³⁺-containing spinel phases, the composition distributions of which obtained from LDHs precursors depend on the nature of interlayer anions, thus resulting in the difference of the reducibility of reducible metal species in the calcined LDHs. Moreover, the surface basicity of the calcined material, which is related to the different behaviour of LDHs precursors during the thermal decomposition depending on the interlayer anions, increases progressively following the order of calcined LDHs from sulfate to nitrate and carbonate.     

2-(1-苯基-1H-四唑-5-硫基)-N-芳基乙酰胺的合成及其生物活性研究

采用微波法通过2-氯乙酰芳胺与1-苯基-1H-四唑-5-硫醇反应合成了一系列2-(1-苯基-1H-四唑-5-硫基)-N-芳基乙酰胺. 其结构经 IR, ¹H NMR, ¹³C NMR 和元素分析表征. 生物活性实验结果表明, 该类化合物在较低浓度下对油菜籽和小麦的生长表现出良好的促进作用.     

投入产出技术在计划平衡中的理论与应用

在用投入产出技术作计划平衡时，目前一般采用最终产品法、总产品法及国民收入法等．本文从理论上研究了这些方法的可行性问题，并在此基础上提出一个较理想的综合法．最后附有实例并说明综合法的现实意义．     

A Highly Convergent Synthesis of 2‐Phenyl Quinoline as Dual Antagonists for NK2 and NK3 Receptors

A novel and highly convergent synthesis leading to 2‐phenyl‐quinolines has been developed. As demonstrated in the preparation of 6‐fluoro‐3‐(3‐oxo‐piperazin‐1‐ylmethyl)‐2‐phenyl‐quinoline‐4‐carboxylic acid [(S)‐1‐cyclohexyl‐ethyl]‐amide (8), the method provides fascile access to this class of analogues via the common intermediate 7.     

三邻氯苄基锡-2-吲哚甲酸酯的合成、谱学性质和晶体结构(英)

The tri(o-chlorobenzyl)tin ester of 2-indolylcarboxylic acid has been synthesized and characterized by elemental analysis, IR and 1H NMR. The crystal structure has been determined by X-ray single crystal diffraction. The crystal belongs to triclinic with space group P1, a=1.020 0(16) nm, b=1.125 9(18) nm, c=1.321(2) nm, α=83.10(2)°, β=67.597(18)°, γ=84.83(2)°, Z=2, V=1.391(4) nm³, D_x=1.565 Mg·m^-3, μ=1.235 mm^-1, F(000)=656, R=0.049 2, wR=0.131 4. In this compound, the central tin atom is rendered four-coordinated in a tetrahedral structure. The resulting structure is a monomer containing Sn-O bond length of 0.205 4(4) nm. CCDC: 236286.