一种新的16金属笼状物[HN(C_2H_5)_3]_4-[Mo_3~VMo_6~(VI)V_7~(IV)O_(40)(PO_4)]·2[N(C_2H_5)_3]的水热合成和结构

报道了一种新的杂多化合物[HN(C_2H_5)_3]_4-[Mo_3~VMo_6~(VI)V_7~(IV)O_(40)(PO_4)]·2[N(C_2H_5)_3]的合成,并用元素分析、EPR、IR谱、及X--射线单晶衍射等手段进行了表征。结果表明,该杂多酸盐属于单斜晶系,空间群P21/n,a=14.0841(3),b=14.2505(3),c=19.6089(3)?b=94.213(1),V=3925.0(1)?,Z=2,Dc=2.171g/cm3,Mr=2566.18,m=2.284mm-1,F(000)=2516,R=0.0477,wR=0.0945.杂多阴离子是1个16金属笼状物,笼中心包含1个PO4四面体客体。     

Synthesis and photochromic properties of 4-[2-(anthracen-9-yl)-5-methyloxazolyl] fulgide

New photochromic fulgide, viz., 4-{1-[2-(anthracen-9-yl)-5-methyloxazol-4-yl]ethylidene}-3-isopropylidenetetrahydrofuran-2,5-dione, with fluorescent properties was synthesized. Studies by electronic, IR, and ¹H NMR spectroscopy and X-ray diffraction demonstrated that this fulgide exists in the Z form. Light irradiation of its solutions at a wavelength of 365 nm causes Z/E isomerization giving rise to the thermally stable cyclic form. The latter is transformed into the starting E isomer under light irradiation at λ = 436 nm. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 97–101, January, 2006.     

3-[N-(4-甲基苯基)氨基羰基]-5-[4-(4-甲酸基苯甲氧基)苯亚甲基]-2,4-噻唑烷二酮的合成

以对甲苯胺和对甲基苯甲酸甲酯为起始原料,经NBS溴化、亲核取代、酸水解和Knoevenagel缩合等6步反应合成了抗细菌生物膜化合物—3-[N-(4-甲基苯基)氨基羰基]-5-[4-(4-甲酸基苯甲氧基)苯亚甲基]-2,4-噻唑烷二酮,总收率57.3％,其结构经1H NMR,ESI-MS和元素分析确证.     

Synthesis of 5-(4-bromophenyl)- and 5-(5-bromothiophen-2-yl)-substituted 3-aryl[1,2,4]triazolo[4,3-c]quinazolines

Russian Chemical Bulletin - A series of [1,2,4]triazolo[4,3-c]quinazolines, bearing 3-positioned p-bromophenyl or 5-bromothiophen-2-yl fragment, was synthesized by oxidative cyclization of the...     

聚[2-甲氧基-5-(4-溴-丁氧基)对苯乙炔]新型前聚物的合成及表征]

采用不同方法由三锍盐合成新型的聚电解质前聚物及可溶于有机溶剂的侧链溴代聚对苯乙炔前聚物,发现侧链烷氧取代基上的锍盐并不参与聚合,所得前聚物加热后都可转化为聚对苯乙炔.光物理初步研究表明,溴代侧链聚对苯乙炔与C₆₀掺杂后具有良好的光电特性.以IR、UV-Vis、¹H NMR、DSC对单体及前聚物进行了表征.     

3-Alkyl-2-[3(4)-pyridyl]-5-(2-vinyloxyethoxymethyl)-oxazolidines

1-Alkylamino-3-(2-vinyloxyethoxy)-2-propanols react with 3-and 4-pyridinecarbaldehydes to give equimolar mixtures of cis- and trans-3-alkyl-5-(2-vinyloxyethoxymethyl)-2-[3(4)-pyridyl]oxazolidines.__________Translated from Zhurnal Organicheskoi Khimii, Vol. 41, No. 1, 2005, pp. 104–108.Original Russian Text Copyright © 2005 by Kukharev, Stankevich, Lobanova, Klimenko, Kukhareva.     

3-[4-(咪唑)苯乙烯基]-9-乙基咔唑的合成及其性质研究

通过固相Wittig反应合成了一种新型含π电子共轭体系的咔唑衍生物——3-[4-(咪唑)苯乙烯基]-9-乙基咔唑(4),其结构经1HNMR,IR,MS,元素分析和X-射线单晶衍射表征。结果表明,4具有较高的热稳定性及优良的光学性质。     

含4-叔丁基环己基和烯烃共轭结构的双苯并噻唑类聚合物的合成及性能

一类新型的含4-叔丁基环己基和烯烃共轭结构的双苯并噻唑类聚合物PBTs III1,2由1,1’-双(4-氨基-3-巯基苯基)-4-叔丁基环己烷二盐酸盐(BAMPBCH?2HCl)与烯烃二元酸经过缩聚反应制备得到。聚合物的结构都经过了红外(IR)、核磁(NMR)、元素分析(EA)的表征。4-叔丁基环己基的引入提高了此类聚合物的溶解性并保持了较好的热稳定性,失重10%的温度在419 oC以上。相比聚苯撑苯并双噻唑(PBZT),PBTs III1,2的紫外吸收波长发生了蓝移,相对聚2,2’-对苯撑-6,6’-(4-叔丁基)环己基双苯并噻唑(PBT)则发生了红移,光学能带隙分别为2.56eV和2.53eV,大侧基和烯烃结构的引入扩大了苯并噻唑类聚合物光学能带隙的可调范围。PBTs III1,2的荧光发射波长较PBT发生了红移,大侧基的引入降低了固态时聚合物分子链的聚集程度。顺磁共振(EPR)的结果表明,PBTs III1,2都有明显的顺磁共振信号,顺磁中心是它们本身所固有的。     

Solvothermal Synthesis and Characterization of [TM(1,2-dap)_3]HgSb_2Se_5(TM = Co,Fe)with a Chain Structure

One organic-decorated quanternaery [TM(1,2-dap)3]Hg Sb2Se5(1,2-dap = 1,2-dianinopropane, TM = Co(1), Fe(2)) compound has been solvothermally synthesized. The compounds crystallize in triclinic space group P 1, with a = 11.248(6), b = 11.542(7), c = 12.180(12) ?, V =1268.7(16) ?~3, Z = 2, F(000) = 1010 for 1 and a = 11.311(5), b = 11.558(5), c = 12.180(9) ?, V =1276.5(12) ?~3, Z = 2, F(000) = 1008 for 2. The crystal structure consists of one-dimensional anionics chains composed of Hg Se4 tetrahedra and SbSe_3 trigonal pyramids sharing corners and[TM(dap)_3]~(2+) cations. The [HgSb_2Se+5~(2-)]∞ anionic chains run along the [001] direction, and are surrounded by the [TM(dap)_3]~(2+) cations. Meanwhile, 8-ring [Hg_2Sb_2Se_4] and 6-ring [HgSb_2Se_2] are alternately found. The compounds were structurally characterized by elemental analysis,thermogravimetric analysis, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy.     

New Dimeric Selenidoarsenate(III):Solvothermal Synthesis and Crystal Structure of [Co(en)_3]_2As_2Se_5

1 INTRODUCTION The mild solvothermal synthesis with the presence of a structure-directing agent is proved to be a versa- tile route for the preparation of chalcogenidometa- lates of the heavier group (14 and 15) elements[1～3]. Templated by the transition metal complex cations, a large number of chalcogenidoantimonates containing transition metal complex ions have been synthesized by solvothermal method, such as Mn2(en)2Sb2S5[4], [Co(en)3]CoSb4S8[5], [M(en)3]Sb2S4 (M = Co, Ni)[6], [N…     

新型Mo-Pb-S异四核簇合物 [Mo~3(PbI~3)S~4(dtp)~3(C~3H~4N~2)~3][(CH~3) ~2CO]~2 的合成和晶体结构

由[Mo~3(μ~3-O)(μ-S)~3(dtp)~4(H~2O)和PbI~3^-在咪唑存在下反应获得异四核混合簇[Mo~3(PbI~3)S~4(dtp)~3(C~3H~4N~2)~3][(CH~3)~2CO]~2(2)[dtp=S~2P(OC~2H~5)~2^-]。簇合物属斜方晶系,空间群P~b~c~a(No.61),晶胞参数为a=2.3590(3),b=1.9161(5),c=2.6458(9)nm,V=11.959(6)nm^3,Z=8。结构最终偏离因子R=0.067。此四核簇分子具有[Mo~3PbS~4]类立方烷簇芯,簇分子整体对称性接近C~3~v。在同一不对称单元中,簇分子的咪唑环以(NH)和溶剂丙酮分子的氧原子形成O---H---N氢键。     

Synthesis and spectral properties of 4-(ortho-R-benzylideneamine)-5-[2-(2-pyridyl)ethenyl]-3-methylisoxazole

The preparation of several 5,4-disubstituted 3-methylisoxazoles is described. The structure of all products was corroborated by ir, ¹H-nmr and mass spectrometry.     

Synthesis and Anticancer Activity Evaluation of 5-[2-Chloro-3-(4-nitrophenyl)-2-propenylidene]-4-thiazolidinones

A series of novel 5-[(Z,2Z)-2-chloro-3-(4-nitrophenyl)-2-propenylidene]-thiazolidinones (Ciminalum–thiazolidinone hybrid molecules) have been synthesized. Anticancer activity screening toward the NCI60 cell lines panel, gastric cancer (AGS), human colon cancer (DLD-1), and breast cancer (MCF-7 and MDA-MB-231) cell lines allowed the identification of 3-{5-[(Z,2Z)-2-chloro-3-(4-nitrophenyl)-2-propenylidene]-4-oxo-2-thioxothiazolidin-3-yl}propanoic acid (2h) with the highest level of antimitotic activity with mean GI₅₀/TGI values of 1.57/13.3 μM and a certain sensitivity profile against leukemia (MOLT-4, SR), colon cancer (SW-620), CNS cancer (SF-539), melanoma (SK-MEL-5), gastric cancer (AGS), human colon cancer (DLD-1), and breast cancers (MCF-7 and MDA-MB-231) cell lines. The hit compounds 2f, 2i, 2j, and 2h have been found to have low toxicity toward normal human blood lymphocytes and a fairly wide therapeutic range. The significant role of the 2-chloro-3-(4-nitrophenyl)prop-2-enylidene (Ciminalum) substituent in the 5 position and the substituent’s nature in the position 3 of core heterocycle in the anticancer cytotoxicity levels of 4-thiazolidinone derivatives have been established     

Synthesis of 1-R-2-amino-3-[2-(benz)azolyl]-4(5H)-ketopyrroles

A study has been made of the interaction of 2-[2-(benz)azolyl]3-keto-4-chlorobutanenitriles with primary aliphatic amines. This is a convenient method for the synthesis of 2-amino-3-[2-(benz)azolyl]-4(5H)-ketopyrroles.Tarasa Shevchenko Kiev University, Kiev 252601, Ukraine; e-mail dov@fosfor.kiev.ua. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 50–57, January, 1998.     

3-[4-(咪唑)苯乙烯基]-9-丁基咔唑的合成及其光学性质

设计并合成了一种含π共轭结构的有机荧光化合物--3-[4-(咪唑)苯乙烯基]-9-丁基咔唑。通过¹HNMR、 ¹³CNMR和IR表征了化合物的结构。采用UV-Vis、荧光光谱和理论计算分析了化合物的光学性质。结果表明：化合物在二氯甲烷(DCM)、乙酸乙酯(EA)、四氢呋喃(THF)、乙醇(EtOH)、乙腈(ACN)、 N,N-二甲基甲酰胺(DMF)和二甲基亚砜(DMSO)中均存在两个吸收峰,其中吸收峰一位于300nm附近,吸收峰二位于335nm附近;在上述溶剂中,λ_em依次为431 nm、 423 nm、 425 nm、 429 nm、 432 nm、 434 nm和439 nm。计算结果显示：第一激发过程属于π→π^*跃迁。     

[M(en)3]2Sn2Se6(M=Mn,Zn)的制备及其热稳定性

用有机溶剂热生长技术(SolvothermalTechnique)制备过渡金属锰和锌硒化物[Mn(en)3]2Sn2Se6(Ⅰ),[Zn(en)3]2Sn2Se6(Ⅱ).用单晶X射线衍射技术对其进行晶体结构分析.[Zn(en)3]2Sn2Se6样品的热分析结果表明,该化合物的热分解分三步进行.光学性质测试表明它们是半导体材料,[Mn(en)3]2Sn2Se6的能带隙为1.76eV.[Zn(en)3]2Sn2Se6的能带隙为2.49eV.     

Recyclization of 5-[methyl(phenyl)amino]-2-(4-nitrobenzyl)-3-p-tolyl-1,2,4-thiadiazolium perchlorate into 9-methyl-3a-(4-nitrophenyl)-2-p-tolyl-3a,9-dihydrobenzo[b]-imidazo[4,5-e][1,4]thiazine

Russian Journal of General Chemistry -     

Molten Salt Synthesis, Crystal Structure and Optical Properties of a Novel Quaternary Metal Selenide, K2AgIn3Se6

K2AgIn3Se6 was synthesized by a molten-salt (alkali-metal polyselenide flux) reaction at 500 ℃. The orange red granular crystal crystallizes in monoclinic space group C2/c with cell parameters, a=1.16411(7) nm, b=1.16348(8) nm, c=2.14179(12) nm, V=2.8740(9) nm^3, and Z=8. The crystal has a new two-dimensional structure containing ^2∞[AgIn3Se6]^2- anionic layers separated by K^- cations and the ^2∞[AgIn3Se6]^2- layer is constructed with corner-shared [AgSe4] and [InSe4] tetrahedra. The optical band gap of K2AgIn3Se6 was determined to be ca. 2.9 eV by UV/vis/NIR diffuse reflectance spectra.     

N,N′-二[3-氯-5S-(l-孟氧基)-2(5H)-4-呋喃酮基]-1,4-丁二胺的合成及晶体结构(英文)

合成了N,N′-二[3-氯-5S-(l-孟氧基)-2(5H)-4-呋喃酮基]-1,4-丁二胺,并通过IR,1H NMR,MS和X射线单晶衍射对其进行了表征.X射线单晶衍射结果表明:标题化合物的不对称结构单元中包含一个平面的呋喃酮环和一个椅式的环己烷环,四个手性中心.标题化合物通过N—H…O分子间氢键作用实现空间堆积.