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1.
采用水热条件合成了1个钴配合物[Co(phen)(HBTC)(H2O)3].2.5H2O(phen=1,10-邻菲罗啉,H3BTC=均苯三甲酸),通过元素分析,红外光谱,紫外光谱,热重分析对其结构和性质进行表征及研究,用X-射线单晶衍射测定了该化合物的晶体结构。晶体属于单斜晶系,空间群为P21/n,晶胞参数a=0.78889(8)nm,b=1.9000(2)nm,c=1.56387(16)nm,β=98.780(2)°,V=2.3166(4)nm3,Z=4。标题化合物的不对称单元由1个配合物分子[Co(phen)(HBTC)(H2O)3]及2.5个结晶水分子组成,氢键将它们连接起来,形成了三维网络结构。利用循环伏安法测定了配合物的电化学性质,并测定了配合物的荧光光谱,发现配合物在383和469 nm两处有发射峰。  相似文献   

2.
采用缓慢蒸发溶剂法在水中合成了2个含双磺酸基的化合物A-2,5-DSA·(Hphen)2·2H2O(1)和[Co(phen)2(H2O)2]·(A-2,5-DSA)·3H2O(2)(A-2,5-DSA=苯胺-2,5-二磺酸根离子,phen=1,10-邻菲罗啉)。化合物1中,相邻的质子化的1,10-邻菲罗啉反向堆叠在一起,水分子通过氢键与(Hphen)+和苯胺-2,5-二磺酸根离子相连,形成二维的层状结构。化合物2中,钴离子与2个1,10-邻菲罗啉和2个水分子配位,构成[Co(phen)2(H2O)2]2+阳离子。3个自由的水分子通过氢键将苯胺-2,5-二磺酸根离子和[Co(phen)2(H2O)2]2+连接形成三维网状结构。两个化合物中苯胺-2,5-二磺酸根离子均起到平衡电荷的作用。室温下2个化合物均具有荧光性质,其最大发射峰分别在601 nm和441 nm。  相似文献   

3.
在水和乙醇的混合体系中合成了2个配位化合物[Co(Bpz*ea T)(H2O)3]·2H2BTC·2H2O(1)和[Cu(Bpz*ea T)(H2O)3]·2H2BTC·CH3CH2OH·H2O(2)[Bpz*ea T=2,4-二(3,5-二甲基吡唑)-6-二乙胺基-1,3,5-三嗪;H3BTC=均苯三甲酸].通过元素分析、红外光谱、紫外光谱、热重分析、X射线粉末衍射以及X射线单晶衍射方法对配合物进行了表征.结构分析表明,配合物1和2的中心金属均为六配位,形成扭曲的八面体构型.通过分子间氢键的作用,配合物1和2分别被连接成三维和二维的超分子结构.此外,对2个配合物的光催化活性进行了研究.  相似文献   

4.
Two new complexes [Mn(DHTA)(PLQ)]n(1) and{[Co2(DHTA)(phen)2(H2 O)6]· DHTA}n(2)(H2 DHTA = 2,5-dihydroxy-1,4-benzenedicarboxylic acid, PLQ = 1,10-phenanthroline-5,6-quinone, phen = 1,10-phenanthroline) have been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, fluorescence spectrum, single-crystal and power X-ray diffraction. Complex 1 exhibits a two-dimensional(2 D) network, which was stabilized through O–H···O hydrogen bonding interactions. Complex 2 shows a zero-dimensional structure, which was further extended into a three-dimensional supramolecular structure through O–H···O hydrogen bonds and π-π interactions.  相似文献   

5.
采用水热法合成了新的配合物[Ni(H2O)6].[Ni2(phen)2(BTC)2(H2O)4].4H2O(phen=邻菲啰啉;BTC=均苯三甲酸),采用X射线单晶衍射结构分析及元素分析、红外光谱等表征,并用TGA检测了该配合物的热稳定性.晶体属于三斜晶系,空间群为P-1,晶胞参数a=0.84038(7)nm,b=0.92048(8)nm,c=1.64793(14)nm,α=97.3850(10)°,β=102.7930(10)°,γ=104.9700(10)°,V=1.17736(17)nm3,F(000)=622,Z=1.标题化合物的不对称结构是由NiO6单元和1个二聚物Ni2N4O12单元组成的,该二聚物单元通过2个邻菲啰啉和2个均苯三甲酸分子构筑了1个八元环.氢键将2个独立的结构单元连接成三维结构.  相似文献   

6.
采用水热法合成了3种以5-氨基间苯二甲酸根为桥连配体的Co(Ⅱ)配聚物:[Co2(aip)2(bipy)]n·2nH2O(1),[Co(aip)(imH)]n(2)和[Co(aip)(phen)]n(3)(H2aip=5-氨基间苯二甲酸,bipy=2,2′-联吡啶,imH=咪唑,phen=1,10-邻菲啰啉).通过X射...  相似文献   

7.
采用水热方法,选用2,3,3',4'-二苯醚四羧酸(H4deta)和2,2'-联咪唑(H2biim)、菲咯啉(phen)分别与CoCl2·6H2O在160℃下反应,得到了具有一维链结构([Co2(μ3-deta)(H2biim)3(H2O)2]n,1)和二维网络结构({[Co2(μ6-deta)(phen)2]· H2...  相似文献   

8.
[CoII(phen)3]2[{(ZnW12O40)CoII(phen)2(H2O)}2CoII(trien)2(NaH2O)2]·3H2O was synthesized via hydrothermal technique and characterized with elemental analyses, IR spectroscopy, TGA-DTA, and variable temperature magnetic susceptibility. The compound crystallized in the monoclinic system with the space group P21/n, a=1.8210 nm, b=2.3592 nm, c=2.2932 nm, β=110.31o, V=9.239 nm3, Z=2, R1=0.0827. The compound consists of two coordination cations, three lattice water molecules, and a macroanion [{(ZnW12O40)Co(phen)2(...  相似文献   

9.
Three new Keggin polyoxometalates, [Zn(phen) 3 ] 2 [SiW 12 O 40 ]·5H 2 O(1), [Co(phen) 3 ] 2 [SiW 12 O 40 ](2) and [Ni(phen) 3 ] 2 [SiW 12 O 40 ]·2H 2 O(3)(phen=1,10′-phenanthroline) have been hydrothermally synthesized and characterized by elemental analysis, IR, crystal X-ray diffraction, thermogravimetric analyses(TGA) and fluorescence techniques. Complex 1, crystallized in the triclinic space group P1, consists of one [SiW 12 O 40 ] 4– anion, two discrete [Zn(phen) 3 ] 2+ cations and five crystal water molecules. Complexes 2 and 3 have the similar configuration to complex 1, but they crystallized in the monoclinic space group C2/c. Variable-temperature magnetic susceptibilities of complexess 2 and 3 reveal antiferromagnetism and ferromagnetism, respectively.  相似文献   

10.
冯秀玲  张玉平 《合成化学》2011,19(5):652-655
以Co( NO3)2.6H2O,邻菲罗啉(phen)与L-丙氨酸(L-alanine)为原料,通过水热法合成了新型超分子化合物[ Co(L-alanato)2(phen)] NO3.4H2O(1),其结构经IR,元素分析和X-射线单晶衍射分析表征.1属三斜晶系,空间群P-1,晶胞参数a=10.121 9(5)(A),b...  相似文献   

11.
用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.  相似文献   

12.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

13.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

14.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

15.
The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.  相似文献   

16.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

17.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

18.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

19.
N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).  相似文献   

20.
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.  相似文献   

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