Reactions of 5-dialkylamino-1,2,3-thiadiazole-4-carbaldehydes with amines as a method for the synthesis of 1,2,3-triazole-4-carbothioamides

A method for the synthesis of previously inaccessible 5-dialkylamino-substituted 1,2,3-thiadiazole-4-carbaldehydes was developed. Ring transformation in these compounds induced by primary aliphatic and aromatic amines, hydroxylamines, and N-substituted hydrazines resulted in the synthesis of a broad range of 1,2,3-triazole-4-carbothioamide.     

Electroreduction of Pd(II) Complexes with α-Alanine on a Palladium Electrode

The kinetics of electroreduction of Pd(II) complexes with -alanine, Pd(ala)₂, is studied on a rotating Pd disk electrode in solutions of pH 8–13 containing large excess of -alanine and various supporting electrolytes (NaF, Na₂SO₄, NaClO₄). On a Pd electrode, complexes Pd(ala)₂ undergo reduction at potentials much more negative than on an Hg electrode. This is attributed to the chemisorption of water on the Pd electrode, which hampers adsorption of Pd(ala)₂ that take part in the slow electrochemical stage. As with the Hg electrode, perchlorate ions hinder the Pd(ala)₂ reduction on a Pd electrode. Studying adsorption of Pd(ala)₂ on a Pd electrode is hampered by parallel processes of hydrogen adsorption and absorption.     

氧缺位铁酸盐的制备及结构与还原行为的研究

在３５８Ｋ下用２００ｍｌ／ｍｉｎ的空气氧化碱性悬浮液合成了ＭＦｅ_２Ｏ_（４＋δ）（δ≥０，Ｍ＝Ｆｅ、Ｃｏ、Ｎｉ、Ｍｎ），并在５７３Ｋ下用４０ｍｌ／ｍｉｎ的Ｈ_２还原ＭＦｅ_２Ｏ_（４＋δ）制备了氧缺位铁酸盐ＭＦｅ_２Ｏ_（４－δ）（δ＞０）。用ＸＲＤ、Ｍｓｓｂａｕｅｒ谱等测试方法对铁酸盐的结构进行了表征，考察了铁酸盐的组成及第二金属组分（Ｃｏ、Ｎｉ、Ｍｎ）对铁酸盐还原性能的影响。在Ｈ_２还原３ｈ内，铁酸盐氧缺位程度随还原时间增加而增大，晶格常数也相应增大；５ｈ以上，铁酸盐将被还原为ＭＯ－ＦｅＯ或α－Ｆｅ，晶格常数几乎不变。按Ｆｅ、Ｃｏ、Ｎｉ、Ｍｎ顺序，ＭＯ与ＦｅＯ的相互作用能力、ＭＯ－ＦｅＯ固溶体的稳定性及铁酸盐还原为ＭＯ－ＦｅＯ的能力均增强，ＭＯ－ＦｅＯ进一步还原为α－Ｆｅ的能力却减弱。     

Reduction of 2,5-di-tert-butylcyclopentadienone and pyridine with thulium diiodide. Structures of the complexes TmI2(THF)2[η5-But2C5H2O]TmI2(THF)3 and [TmI2(C5H5N)4]2(μ2-N2C10H10)

Reduction of 2,5-di-tert-butylcyclopentadienone with two equivalents of thulium diiodide in tetrahydrofuran afforded the binuclear thulium(iii) complex with the cyclopentadienyl oxide ligand, viz., TmI₂(THF)₂[⁵-Bu^t ₂C₅H₂O]TmI₂(THF)₃ (1). Shielding of the carbonyl carbon atom with two tert-butyl substituents prevents pinacolization of the ketyl radical anions that formed upon one-electron reduction of cyclopentadienone. The reaction of thulium diiodide with an excess of pyridine in tetrahydrofuran gave a product of reductive coupling of two pyridine radical anions, viz., [TmI₂(C₅H₅N)₄]₂(₂-N₂C₁₀H₁₀) (2). The structures of complexes 1 and 2 were established by single-crystal X-ray diffraction analysis.     

工科学校本科生科研训练与实践——以节能减排大赛为例

Scientific research training is an essential part of undergraduate learning, which plays an important role in improving students' knowledge utilization and scientific literacy. Taking the participation process of "Energy conservation and emission reduction competition" as an example, this paper briefly introduces the undergraduate scientific research training of students majoring in polymer materials and engineering from their own perspective, and the way to combine the discipline and school characteristics to reflect the thinking of engineering students in scientific research and practical application.     

An expedient preparation of Stryker's reagent

A convenient and efficient preparation of Stryker's reagent, [Ph₃PCuH]₆, under homogeneous conditions using silanes as the reducing agent is detailed. The reaction time can be reduced to 1-2 h, and high yields of Stryker's reagent can be routinely achieved. The same method has been extended to the synthesis of [Ph₃PCuD]₆ using Ph₂SiD₂.     

Crystal Structure of (6S,9S,13R,14S)-7,8-Didehydro-3,7-dimethoxy-17-methylmorphinan-4,6-diol

1 INTRODUCTION (9S,13R,14S)-7,8-Didehydro-3,7-dimethoxy-4-hydroxy-17-methylmorphinan-6-one I is an impor- tant natural product that was used to ease pain, decrease blood pressure and diminish inflammation. In order to study the stereochemistry of the reduction of I with potassium boronhydride, the crystal structure of the title compound II was determined by X-ray diffraction method. 2 EXPERIMENTAL 2. 1 Instrument The melting point was measured on a Yanagimoto MP-500 apparatus…     

Heterometallic zirconocene(iii) aluminum hydride complex (Cp2ZrH)2HAlCl2·C4H8O2·C6H6

The heterometallic zirconocene(iii) aluminum hydride complex (Cp₂ZrH)₂HAlCl₂·C₄H₈O₂·C₆H₆ was synthesized by reduction of Cp₂ZrCl₂ with lithium aluminum hydride in the presence of Cp₂TiBH₄ and 1,4-dioxane, and its structure was established by X-ray diffraction analysis.     

酶促酮酸酯还原合成(S)-2乙酰氧基十三烷

Bartelt等 [1] 于 1 989年首次从穆勒果蝇 (Drosophila mulleric)的雄性成虫体内分离出其聚集信息素 ,并确证其主要生物活性的成分为 (S) -构型的 2 -乙酰氧基十三烷 (1 ) ,而 (R) -构型无生物活性 .1 999年Hillbur等 [2 ,3 ] 发现碗豆瘿蚊 (Contarinia pisi)的雌性性信息素主要成分中也含有 (1 ) ,其对碗豆瘿蚊雄虫具有很强的性引诱作用 .有关 (1 )的合成报道较多的为酶促反应合成法 [4～ 7] .我们曾以 1 -苯砜基 - 2 -丙酮为原料经酶促还原反应合成了目标产物 ,此法尽管合成路线短 ,光学产率较高 ,但反应原料不易购得 ,且使用两摩尔比…     

[Co（H2o）4（NCS）2]（18—C—6）的薄层光谱电化学研究

利用光谱电化学方法来研究冠醚类化合物的文章尚未见报导.本文在测定用凝胶法合成的[Co(H_2O)(NCS)_2](18-C-6)的核磁共振谱和红外光谱的基础上,使用循环伏安法和薄层光谱电化学技术,在金微栅电极上测定了此配合物在乙腈溶剂中的第一步克式量电势(E~0′)和电子转移数(n),并推测了电还原反应机理.