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1,3-二苯基-2-吡唑啉-5-酮(1)对查而酮(苯丙烯酰苯,2)的碱性催化加成,生成相应的Michael加成物,4-[α-(苯甲酰甲基)苄基]-1,3-二苯基-2-吡唑啉-5-酮(3),3在沸醇中经肼或羟胺处理得腙或肟(4),4经沸乙酸处理生成1和2的吡唑啉衍生物(5)的混合物,3的还原产物为相应的仲醇(6a~c).Grignard试剂与3反应生成叔醇(6d~1),新化合物的结构经元素分析,IR,~1H和~(13)C NMR证明。 相似文献
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1-苯基-3-甲基-5-吡唑啉酮与二羰基化合物的固相反应研究 总被引:1,自引:0,他引:1
报道了苯偶酰及其衍生物、对二甲氨基苯偶姻、邻苯二甲酰亚胺与1-苯基-3-甲基-5-吡唑啉酮的固相热反应研究;这个热反应以较高的选择性生成1:1缩合产物的一种异构体,通过IR、1HNMR、MS和元素分析确定了新产物的结构,并通过X射线衍射分析确定了其中一个产物的构型。 相似文献
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Villemin[1]曾报道KSF/蒙托土催化下微波促进1-苯基-3-甲基-5-吡唑啉酮(1)与醛2的缩合反应,李晓陆[2研究了该反应的固相缩合,Sun[3]报道了KF-Al2O3催化下甲醇溶液中的反应.本文采用绿色合成原则,无催化剂条件下无溶剂微波辐射及水中回流方法研究了此反应,得到两类化合物(图1).产物结构经1H NMR,13C NMR,MS及IR确证.实验发现辐射功率对产物有很大影响,高辐射功率下得到4-芳甲叉-3-甲基-1-苯基-5-吡唑啉酮(3),低辐射功率得到4,4′-芳甲叉-双(3-甲基-1-苯基-5-吡唑啉酮)(4);水相反应同时得到两种产物,以产物3为主(表1).产物结构与反应物配比无关. 相似文献
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我们在合成1-甲基-3,5-二苯基吡唑(MDPP)的过程中,发现氯化铜、氯化钴等化合物对1-甲基-3,5-二苯基吡唑啉(H2MDPP)的氧化脱氢反应具有优异的催化性能,对以氯化铜为催化剂的反应机理进行了初步研究,获得了反应过程中形成铜(Ⅱ)H2MDPP、铜(Ⅱ)MDPP和铜(Ⅱ)H2MDPP分子氧配合物的证据。另外,在催化氧化反应体系中曾检测到一价铜,这显然是氯化铜的还原产物,故本文对氯化铜与H2MDPP的计量反应及在催化反应中氧分子参与作用的阶段进行了研究。 相似文献
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以水合肼和硝酸胍为原料,经过环合、氧化和肼化,得到3-(3,5-二甲基-1H-吡唑-1-基)-6-肼基-1,2,4,5-四嗪(4),以此为原料和不同芳香醛发生腙化反应,得到系列1-芳基亚甲基-2-(6-(3,5-二甲基-1H-吡唑-1-基)-1,2,4,5-四嗪-3-基)肼(5),产物经元素分析、1H NMR、IR和MS表征。所合成的系列化合物抗菌活性测试表明,它们对大肠杆菌、金黄色葡萄球菌、枯草杆菌等3种细菌表现出一定程度的抑制活性。 相似文献
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The reaction of lanthanum(Ⅲ) nitrate and 5-nitroisophthalic acid in isopropanol/H2O under hydrothermal conditions leads to a 3D lanthanum-containing coordination polymer with the general chemical formula {[La6(Nip)9(H2O)4 ]·(H2O)4 }∞(1,Nip=5-nitroisophthalate).The single-crystal X-ray analyses show that this compound crystallizes in the orthorhombic system,space group Ima2 with a=9.7769(12),b=28.239(3),c=21.149(2),V=5839.1(11)3,Z=2,Mr=2859.61,Dc =1.626 g/cm 3,F(000)=2752.14040 reflections are collected,of which 5275 are unique (R int=0.0241).Final GOOF=1.083,R=0.0406 and wR=0.1182,R indices based on 5183 reflections with I>2σ(I)(refinement on F2),443 parameters,1 restraint.Lp and absorption corrections were applied,=2.242mm-1.Absolute structure parameter x=0.08(3).The crystal structure can be described as the butterfly-liked hexanuclear lanthanum entities {La6O6(CO2)8 } covalently linked to each other by nitroisophthalate ligands into an intricate three-dimensional structure.The fluorescence spectroscopy of compound 1 has been investigated. 相似文献
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A new cyano-bridged GadoliniumⅢ-IronⅢ complex {[Gd(DMF)3(DMSO)(H2O)3](μ-CN)[Fe(CN)5]}·2H2O (DMF=N,N-dimethylformamide; DMSO=dimethylsulfoxide) was synthesized by the grinding reaction method. It crysta-llizes in the triclinic, space group P1 with cell parameters: a=0.90363(2) nm, b=1.250 78(3) nm, c=1.41303(1) nm, α=93.174(1)°, β=94.406(1)°, γ=91.817(2)°, and V=1.588 87(5) nm3, Dc=1.582 g·cm-3, Z=2, Mr=756.72, F(000)=760, μ=2.645 mm-1. The slightly distorted square-antiprism eightfold-coordinated Gd(Ⅲ) and the approxi-mately oriented octahedrally sixfold-coordinated Fe(Ⅲ) are linked by a cyano-bridge group to construct a dinuclear compound. The {[Gd(DMF)3(DMSO)(H2O)3](μ-CN)[Fe(CN)5]} species are held together via hydrogen bonds to form a three-dimensional framework. The Gd(Ⅲ)-Fe(Ⅲ) interaction is antiferromagnetic. CCDC: 223430. 相似文献
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JIANG Yin-Zhi ZHANG Lian-Qun ZHAO Jian-Min QIN Men-Yun 《结构化学》2007,26(6):737-741
In order to continue our studies on the synthesis, properties and coordination of s-tetrazine, 3,6-di-(pyridin-3-yl)-s-tetrazine (II, 3-dptz) was synthesized and characterized by 1H- NMR, MS and IR spectra. And the coordination reaction of 3-dptz with nitrate of Cu(II) was studied. 3-dptz reacting with CuII salt [Cu(NO3)2·2H2O] generates a new salt, nitrate of 2,5-di-(pyridin-3- yl)-1,3,4-oxadiazolene (III). III was determined by IR spectra and single-crystal X-ray diffraction to give the following crystal data: space group P21/c, a = 4.9112(1), b = 8.4101(3), c = 29.499(1) , β = 93.266(2)o, V = 1216.44(7) nm3, Mr = 287.24, Z = 4, Dc = 1.568 g/cm3,μ= 0.122 mm-1, F(000) = 592, R = 0.0430 and wR = 0.1240. The results show that III is composed of one cation and one nitrate anion. The cation consists of one H+ and one 2,5-di-(pyridin-3-yl)-1,3,4-oxadiazol molecule, with the former being attached to the latter via electrovalent bond with N3 atom. And the O(42) atom in the nitrate anion is disordered. Intra- and intermolecular H-bonds are observed in the crystal of the title compound. The mechanism of metal-assisted decomposition was also discussed briefly. 相似文献
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为了模拟植物光系统的给体部分,设计、合成了配合物2.在该模型化合物中,配体的邻位被2个{[2-羟基-3-(吗啉基-4-甲基)-5-叔丁基-苄基](吡啶-2-甲基)胺基-甲基}取代的苯酚通过酰胺键与光敏体[Ru(bpy)3]2+共价相连.利用ESI-MS和1D,2DNMR(gCOSY,HSQC和HMBC)对化合物结构进行了鉴定,并通过UV-Vis、荧光发射光谱、闪光光解及电化学对其光化学性能和氧化还原特性进行了研究.结果表明,化合物的吸收波长发生红移;激发态寿命长;可螯合双核高价Mn()原子;且Ru3+/Ru2+的氧化电位比Phenol+/Phenol和Mn(,)/Mn()的高,满足自然界PS电子转移的基本要求,可用于PS给体部分的初步研究. 相似文献
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WANG Yong-Jinga b ZHANG Han-Huia b② HUANG Chang-Canga b YU Xiao-Honga SUN Qiao-Zhena SUN Rui-Qinga a 《结构化学》2004,(8)
1 INTRODUCTION As a rich remarkable class of inorganic cluster systems, polyoxometalates continue to be the focus of significant attention in the 21th century because of their various and alluring topologies as well as their unusual physicochemical prope… 相似文献
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合成了一个新配合物[Mn(napn)(CH3OH)2]ClO4 (C26H26 Cl N2O8Mn,Mr = 584.88,H2napn = 双a-萘酚醛缩乙二胺),并测定了其晶体结构。晶体属于三斜晶系,空间群P ,a = 7.813(1),b = 13.025(2),c = 14.089(2) ? = 64.89(3), = 83.98(3), = 78.11(3)海琕 = 1270.16 ?,Z = 2, Dc = 1.529 g/cm3, F(000) = 604, R = 0.0837, wR = 0.1636。锰(Ⅲ)离子的配位构型为拉长的八面体。Schiff碱配体napn2-中的N2O2在赤道平面与锰(Ⅲ)形成四配位,2个CH3OH中的O原子分别在赤道平面两侧轴向位置与锰(Ⅲ)配位。由于Jahn-Teller效应,轴向上的MnO平均键长为2.52 拧A硗猓О写嬖诜肿幽诤头肿蛹淝饧? 相似文献
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Synthesis and reactivity of 3-(trichlorogermyl)propanoic acid and 3-(triphenylgermyl) propanoic acid
3-(Trichlorogermyl)propanoic acid (la) reacts with phenylmagnesium bromide in malar ratio 1:4 to give 3-(triphenylgermyl)propanoic acid (2a).In the compounds la and 2a theβ-carboxylic functional group shows some unusual properties when they react with excess of phenylmagnesium bromide.The compound la reacts with phenylmagnesium bromide in molar ratio 1:5 to give phenyl 2-(triphenylgermyl)ethylketone (3a) and in molar ratio 1:6 to give l,l-diphenyl-3-(triphenylgermyl)propanol (4a).The compound 2a reacts with phenylmagnesium bromide in molar ratio 1:2 to give 3a and in molar ratio 1:3 to give 4a also.Dehydration of the compound 4a with dilute hydrochloric acid seems especially easy.Moreover,the compound la reacted with phenylmagnsium bromide in molar ratio 1:6,then the mixture was treated with dilute hydrochloric acid to give 1,1-diphenyl-3-(triphenylgermyl)-1-propene (5a) in one pot reaction.Alkyl Ge-C bond in the compound 5a can be cleaved selectively by lithium aluminium hydride ( LiAlH4) in good yiel 相似文献
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报导4-氟-3-羟基-1-取代苯基-6-哒嗪酮及其衍生物的合成,氟代顺丁烯二酸酐和取代苯肼类反应的研究结果及部分化合物的药理实验结果。 相似文献
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三维稀土配位聚合物[Ce2(H2btc)(btc)(H2O)2]n的水热合成与晶体结构 总被引:1,自引:2,他引:1
含有稀土元素的无机一有机配位聚合物因在光、电、磁及催化等方面具有潜在的应用价值而引起人们的关注.芳香多羧基有机配体在合成配位聚合物和多维超分子研究领域中扮演着重要角色.1,2,4,5-均苯四甲酸(H4btc)由于具有独特的配位能力(btc^4-最多可作为八齿配体)和空间特性, 相似文献
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报道标题化合物La(PMBP)_3(H_2O)_2,Hpmbp=C_(17)H_(14)N_2O_2的合成及晶体结构,晶体属于单斜晶系,空间群C2/c,晶体学数据:a=24.744(5),b=16.325(6),c=25.871(5),β=105.44(3)°,V=10073(2)3,M_r=1006,Z=8,D_x=1.328g/cm~(-3),μ=9.042cm~(-1),F(000)=4094。最终偏离因子R=0.049,R_w=0.059。分子中La(Ⅲ)与8个氧原子配位形成三角十二面体构型,La-O平均键长为2.496(2)。 相似文献