4-巯基-4-脱氧-4′-去甲表鬼臼毒素的立体控制合成

4-巯基-4-脱氧-4′-去甲表鬼臼毒素是合成4位硫取代的4′-去甲表鬼臼毒素的关键中间体,由4′-去甲表鬼臼毒素与硫化氢在BF_3·Et_2O存在下立体控制制备,也可通过以NH_3/CH_3CN选择性地水解4-乙酰硫基-4-脱氧-4′-去甲表鬼臼毒素而制备.     

4-(4-吗啉)哌啶盐酸盐的合成

4-甲酸乙酯哌啶与溴苄反应,再经酰胺化和氨化反应制得关键中间体4-氨基-1-苄基哌啶(5);5与2,2-二溴二乙醚经环化反应制得N-苄基-4-(4-吗啉)哌啶,再经成盐,加氢合成了4-(4-吗啉)哌啶盐酸盐(1,总收率24.9%),1的结构经1HNMR,IR和GC-MS确认。     

4-乙酰基-2-硝基苯甲醛的简便合成

从4-乙酰基-2-硝基甲苯出发, 经溴化、羟化、氧化以88.5%的总收率制备得到4-乙酰基-2-硝基苯甲醛.     

4-氨基-4'-氰基联苯的合成

氨基氰基联苯;4-氨基-4'-氰基联苯的合成     

4-（4′-丙基环己基）环己醇的合成

钌／碳催化剂应用于4-(4′-丙基环己基)苯酚(3PCO)的加氢反应，合成了4-(4′-丙基环己基)环己醇。以环己烷为溶剂，在98℃／2MPa，3PCO的转化率为100．0％，催化剂可以重复使用两次。     

2-烷硫基-5-苯基亚甲基-4H-咪唑啉-4-酮的合成与表征

用2-硫代-3-正丁基-5-苯基亚甲基4-咪唑啉二酮的-S-烷基化反应合成了2-烷硫基-3-正丁基-5-苯基亚甲基-4H-咪唑啉-4-酮衍生物。探讨了S-烷基化反应的反应条件和所合成化合物的波谱性质。目标产物均为新的化合物，其结构经元素分析，IR，1H NMR和MS确正。     

反-4-苯基环己醇的合成

以Ranny-Ni为催化剂,于50℃,0.5 MPa～1.0 MPa下在乙醇中催化氢化4-苯基苯酚制备反-4-苯基环己醇,选择性39.89%,分离产率35.15%。     

卤代-2-(3-甲基-5-取代-4H-1,2,4-三唑-4-基)-苯甲酸的合成

邻氮基苯甲酸;缩合反应;卤代-2-(3-甲基-5-取代-4H-1;2;4-三唑-4-基)-苯甲酸的合成     

3-取代-6-甲氧基-7-羟基-4Н-色烯-4-酮的合成及其异常反应

报道了3-位分别为苯基、氢原子以及卤素等不同取代的4Н-色烯-4-酮类化合物的合成方法,并探讨和阐明了一些意外产物的获得机理,不仅对该位点的进一步结构改造提供了物质基础,同时拓展了构建4Н-色烯-4-酮类化合物的底物结构.     

Synthesis and mesomorphic properties of 4-(4-bromopropyloxy)-4’-(4-alkyloxybenzylidene)anilines

This article describes the preparation and liquid crystalline properties of a new homologous series of 4-（4-bromopropyloxy）-4’- （4-alkyloxybenzylidene）anilines in which the phenyl ring is armed by a bromopropyloxy chain.The thermal behavior and mesomorphic properties of the synthesized compounds were studied with particular attention given to the correlation between their phase transition temperatures and anisotropic change influenced by molecular structure.All the members displayed enantiotropic smectic phase except for the homologue with the longest alkyloxy chain(R = C₁₈H₃₇),exhibiting only monotropic characteristic. The presence of bromine atom from the propyloxy side chain is found to be capable of altering and influencing the mesomorphic properties.     

The crystal structure of LaIr4B4, ThOs4B4, ThIr4B4 (NdCo4B4-type) and URu4B4, UOs4B4 (LuRu4B4-type)

The crystal structure of LaIr₄B₄ has been refined from single crystal counter data. LaIr₄B₄ is tetragonal,P4₂/n,Z=2, isotypic with NdCo₄B₄, |F|/|F _o|=0.039 for 312 independent reflections [|F _o|>2 (F _o)]. ThIr₄B₄ and ThOs₄B₄ also belong to the NdCo₄B₄-type structure. URu₄B₄ and UOs₄B₄ were found to crystallize with LuRu₄B₄-type structure. The crystal chemistry of (RE)T ₄B₄-phases is discussed and simple geometric relations are shown to exist between them.Dedicated to Prof.B. T. Matthias in celebration of his 60th birthday.     

Schwingungsspektren von As4S4 und As4Se4

Vibrational Spectra of As₄S₄ and As₄Se₄ The vibrational spectra of solid α- and β-As₄S₄ and the Raman spectrum of molten As₄S₄ have been recorded. The assignments of the frequencies are proposed mainly based on polarization data. The Raman melt spectra suggest that As₄S₄ molecules (symmetry D_2d) are retained in the molten state. A partial decomposition of the melt by prolonged laser irradiation was observed. The Raman spectrum of solid As₄Se₄ is presented and the frequencies are tentatively assigned to an As₄Se₄ molecule of the cradle type, possessing D_2d symmetry.     

Electronic structures of the boron cage molecules B4H4, B4Cl4 and B4F4

Ab initio calculations have been performed on B₄H₄, B₄Cl₄ and B₄F₄ in order to aid our understanding of the bonding in these compounds, which is presumably based on a tetrahedral boron cage. This cage has only 8 electrons and so is less than that expected on the basis of the usual framework electron counting rules. Basis sets with polarisation functions were used at the SCF, CI and CPF levels of theory to confirm that the T _d structures are indeed more stable than the D _4h ones. Davidson-Roby population analyses were able to show that many factors, including 3-centre 2-electron bonding and backbonding from the ligand to the boron cage, are of importance in determining the relative stability of the three compounds, of which B₄Cl₄ is the only one that has yet been observed experimentally.     

Zintlphasen mit isolierten SiAs4- bzw. GeAs4-Anionen: Darstellung und Struktur von Ba4SiAs4 und Ba4GeAs4 sowie Sr4SiAs4 und Sr4GeAs4

Die erstmals dargestellten isotypen Verbindungen Ba₄SiAs₄, Ba₄GeAs₄, Sr₄SiAs₄ und Sr₄GeAs₄ kristallisieren kubisch, Raumgruppe P4 3n, mit 8 Formeleinheiten in der Elementarzelle: In den Strukturen liegen isolierte, d.h. nur von Ba-Ionen umgebene SiAs - bzw. GeAs -Tetraeder vor. Die Verbindungen sind die bisher eindrucksvollsten Beispiele für Zintlphasen mit komplexen Anionen. Zintl Phases with Isolated SiAs₄ or GeAs₄ Anions: Preparation and Structure of Ba₄SiAs₄, Ba₄GeAs₄, Sr₄SiAs₄, and Sr₄GeAs₄ The new compounds Ba₄SiAs₄, Ba₄GeAs₄, Sr₄SiAs₄, and Sr₄GeAs₄ have been prepared and their structures determined. They crystallize in the cubic system, P4 3n, with axes: data see “Inhaltsübersicht”. There are isolated SiAs or GeAs tetrahedra in the structures. The compounds can be interpreted as Zintl phases with complex anions.     

Zur Kenntnis von K4PbO4 und Rb4PbO4

On K₄PbO₄ and Rb₄PbO₄ For the first time single crystals of K₄[PbO₄] have been prepared by heating K₄PbO₃ in O₂. The structure has been refined [K₄[PbO₄]: 3029 I₀(hkl), four circle diffractometer PW 1100, ω-scan, MoKα, R = 6.73%, R_w = 6.64%, P1 ; a = 658.62(15), b = 658.41(12), c = 986.64(21) pm, α = 79.74(2)°, β = 108.45(2)°, γ = 112.49(2)°, d_x = 3.79 g · cm^?3, d_pyk = 3.78 g · cm^?3, Z = 2; Rb₄[PbO₄]: a = 686.94(18), b = 684.43(18), c = 1020.73(21) pm, α = 79.28(2)°, β = 108.40(2)°, γ = 113.02(2)°, d_x = 4.87 g · cm^?3, d_pyk = 4.85 g · cm^?3, Z = 2, (from Rb₂PbO₃ and Rb₂O)]. Both compounds are isotypic with K₄SnO₄. The Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.