共查询到18条相似文献,搜索用时 171 毫秒
1.
N-芳基-N'-[(4-吡啶基)羰基]氨基硫脲用85%的水合肼环化, 得到3-(4-吡啶基)-4-氨基-5-芳氨基-1,2,4-三唑(2a~2c). 然后再与3-甲酰基色酮(3a~3d)反应, 制备得到了一系列新化合物: 3-(4-吡啶基)-4-(6-取代色酮-3-基亚甲氨基)-5-芳氨基-1,2,4-三唑(4a~4c, 5a~5c, 6a~6c, 7a~7c). 化合物的结构经元素分析, IR, 1H NMR和MS确证. 相似文献
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以2-氨基-5-取代苯氧甲基-1,3,4-噻二唑(1)为起始原料, 合成了中间体2-氯乙酰氨基-5-取代苯氧甲基-1,3,4-噻二唑)-2-乙酰亚胺(2)和2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-4-噻唑啉酮(3), 化合物3进一步与取代苯甲醛发生类Knoevenagle缩合反应, 得到了一系列2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-5-(取代苯基亚甲基)-4-噻唑啉酮类化合物4a~4p. 目标化合物4a~4p的结构经IR, 1H NMR和元素分析确证. 相似文献
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超声辐射下合成1-[(未)取代苯酰基-3-[5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑-2-基]-硫脲 总被引:2,自引:0,他引:2
1-苯基-3-甲基-5-氯吡唑-4-甲酸与氨基硫脲在三氯氧磷中反应得到2-氨基-5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑(1), 然后分别采用超声辐射法和常规加热法与(未)取代苯甲酰基异硫氰酸酯(2)反应合成了一系列未见报到的1-[(未)取代苯酰基-3-[5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑-2-基]-硫脲(3a~3j). 化合物的结构经元素分析, IR, 1H NMR确证. 相似文献
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糖基异硫氰酸酯(1a~1c)与无水肼反应, 生成糖基氨基硫脲2a~2c, 再与6-取代-3-甲酰基色酮3a~3d反应, 得到一系列新的N-糖基-N-(6-取代色酮-3-基-亚甲氨基)硫脲类化合物4a~4d, 5a~5d, 6a~6d. 所有新化合物的结构均经IR, 1H NMR, MS谱和元素分析证实. 所得糖的衍生物构型保持不变, 均为β-型. 相似文献
6.
1-[5-(1,3-二氧-4,5,6,7-四氢-1H-异吲哚-2-基)苯基]-3-取代脲衍生物的合成与除草活性研究 总被引:1,自引:0,他引:1
为了寻找高效低毒的原卟啉原氧化酶抑制剂(protox)类除草剂, 设计并合成了一系列1-[5-(1,3-二氧-4,5,6,7-四氢-1H-异吲哚-2-基)苯基]-3-取代脲类衍生物4a~4d和5a~5g. 化合物4a~4d经异氰酸酯法合成, 收率、纯度高; 化合物5a~5g利用固体光气一锅法合成, 反应时间短.所得化合物结构经1H NMR, IR, 质谱和元素分析表征. 初步生物活性测试表明: 化合物4c, 5a, 5b, 5c在有效成分75 g/hm2 剂量下对苘麻、马刺苋、凹头苋等双子叶杂草表现出90%以上的防效. 相似文献
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为了寻找新的含噻唑杂环的先导化合物, 利用2-取代-1,3-噻唑烷1与氯甲酸取代苯基酯2及取代苯基甲酰氯4在三乙胺存在下发生缩合反应, 合成了6个2-取代-1,3-噻唑烷-3-甲酸酯类化合物3和5个N-苯甲酰基-2-取代-1,3-噻唑烷类化合物5, 并利用1H NMR, IR, MS, 元素分析对其结构进行了表征. 用X-ray单晶衍射测定了2-硫代-1,3-噻唑烷-3-甲酸苯酯(3d)和N-苯甲酰基-2-氧代-1,3-噻唑烷(5a)的晶体结构, 证实了氯甲酸酯与2-硫代-1,3-噻唑烷的反应产物为硫酮式结构, 而非硫酯式结构. 初步生物活性试验结果表明, 在试验浓度下部分目标化合物3和5具有一定的杀菌和杀虫活性. 相似文献
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4-氨基-5-吡啶-4-基-均三唑硫醇(1)在复合催化剂DMAP和TBAB作用下与对卤代苯甲酸经环缩合反应以高收率得到中间体6-(5-氯-3-甲基-1-取代苯基-1H-吡唑-4-基)-3-吡啶-3-基-均三唑并[3,4-b][1,3,4]噻二唑(2a~2c), 接着苯环卤原子与取代哌嗪在聚乙二醇催化作用下发生亲核取代反应得到相应的哌嗪游离碱(3a~3c). 其中, 单取代哌嗪游离碱3a与含功能基的卤代物缩合得到功能基取代的哌嗪衍生物(4a~4g). 这些产生的游离碱与盐酸反应得到相应的水溶性盐酸盐. 所合成新化合物的结构经元素分析和光谱数据表征, 并评价了它们的体外抗菌活性及构效关系. 相似文献
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Some 5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazine-7,9-(6H,8H)-diones (4 a–d) have been synthesised by the condensation of 3-alkyl-4-amino-5-mercapto-(1,2,4)-triazoles (1 a–d) with 5-bromobarbituric acid (2a). Similarly some 9a-nitro-5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazine-7,9(8H,9aH)-diones (5 a–d) have been obtained by the condensation of1 a–d with 5-bromo-5-nitrobarbituric acid (2b) and final cyclisation withPPA. The structures have been confirmed by PMR spectra and analytical results.
Pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazin-7,9(6H,8H)-dione
Zusammenfassung Es wurden einige 5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazin-7,9(6H,8H)-dione (4 a–d) mittels Kondensation von 3-Alkyl-4-amino-5-mercapto-(1,2,4)-triazolen (1 a–d) mit 5-Brombarbitursäure (2 a) dargestellt. Des weiteren wurden einige 9a-Nitro-5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazin-7,9(8H,9aH)-dione (5 a–d) über die Kondensation von1 a–d mit 5-Brom-5-nitrobarbitursäure (2 b) und anschließender Cyclisierung mitPPA synthetisiert. Die angeführten Strukturen wurden mittels PMR-Spektren und analytischen Daten abgesichert.相似文献
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《Journal of Coordination Chemistry》2012,65(22):4038-4054
Four mononuclear copper(II) complexes of two new carboxamide derivatives formulated as [Cu(L1)2](ClO4)2 (1a), [Cu(L1)2](NO3)2 (1b), [Cu(L2)2(H2O)2](ClO4)2 (2a), and [Cu(L2)2(H2O)](NO3)2 (2b) have been isolated in pure form from the reaction of L1 and L2 [where L1 = N-(furan-2-ylmethyl)-2-pyridinecarboxamide and L2 = N-(thiophen-2-ylmethyl)-2-pyridinecarboxamide] with copper(II) salts of perchlorate and nitrate. All the complexes were characterized by physicochemical and spectroscopic tools along with single-crystal X-ray diffraction studies. The structural analyses showed that 1 is monomeric of square planar geometry with copper(II) chelated by two L1 ligands. Complex 2 differs in coordination geometry, being octahedral and distorted square pyramidal. Two L2 ligands occupy the equatorial positions of the octahedral 2a and the basal sites of the pyramidal 2b, with water molecules that complete the coordination sphere in each case. Electrochemical studies using cyclic voltammetry showed a reversible redox behavior of the copper(II) in 1 and 2. The electronic spectroscopic behavior and the trend of one electron equivalent redox potential corresponding to a CuII/CuI couple have also been confirmed by density functional theory calculations. The spectroscopic and viscosity measurement study in tris–HCl buffer suggested an intercalative interaction of 1a and 2 with calf thymus DNA likely due to the stacking between the non-coordinated furan and thiophene chromophore with the base pairs of DNA. 相似文献
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《Journal of Coordination Chemistry》2012,65(4):275-281
This article reports the synthesis and crystal structures of two new mononuclear Zinc(II) complexes, [Zn2(NTB)2(N3)2](NO3)2·2CH3OH (1) and [Zn2(NTB)2(SCN)2](NO3)2·2CH3OH·H2O (2). Complex 1 crystallizes in the triclinic system, space group P&1macr;, a=13.743(4), b=14.374(4), c=14.443(5) Å; α=77.053(5), β=81.824(5), γ=88.959(6)°; Z=2; R1=0.0418, wR2=0.0889. Complex 2 also crystallizes in the triclinic system, space group P&1macr;, a=12.203(10), b=14.430(12), c=18.541(15)Å; α=72.712(15), β=85.039(15), γ=73.610(14); Z=2; R1=0.0771, wR2=0.1288. In both cases the central zinc(II) metal ions are coordinated to the four nitrogen atoms of NTB and a nitrogen atom of N- 3(1) or SCN-(2) to form distorted trigonal bipyramidal coordination spheres. 相似文献
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《Journal of Coordination Chemistry》2012,65(13):2086-2094
Two d10 transition-metal complexes having racemic and enantiomeric 1,2,2-trimethylcyclopentane-1,3-diamine ligands, [Zn(La)2](NO3)2 · CH3CH2OH (1) and [Cd(Lb)2Cl](ClO4) (2) (La = D,L-1,2,2-trimethylcyclopentane-1,3-diamine, Lb = D-(+)-1,2,2-trimethylcyclopentane-1,3-diamine or (1R,3S)-1,2,2-trimethylcyclopentane-1,3-diamine), were synthesized and characterized by X-ray single-crystal diffraction. They crystallize in the Pbca and P212121 space groups, respectively, and have different coordination numbers and coordination geometry (four-coordinate tetrahedron for Zn(II) in 1 and five-coordinate square-based pyramid for Cd(II) in 2) mainly due to their different ionic radii. 相似文献
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《Journal of Coordination Chemistry》2012,65(10):1774-1784
Coordination abilities of unsymmetrical tridentate ligands, 3,3′-polymethylene-2-(pyrid-2′-yl)-benzo[b]-1,10-phenanthrolines (4) were studied. Reactions of the 3,3′-di- and 3,3′-trimethylene-2-(pyrid-2′-yl)benzo[b]-1,10-phenanthrolines (4b and 4c) with RuCl3 ? 3H2O afforded [Ru(4b)2]2+ and [Ru(4c)2]2+ in 57% and 78% yield, respectively, while reactions of the parent non-bridged ligand (4a), tetramethylene-bridged ligand (4d), and fully aromatized ligand (4e) afforded a messy mixture. Reactions of 4 with Ru(tpy)Cl3 (tpy = 2,2′;6′,2″-terpyridine) afforded [Ru(tpy)(4)]2+ in 61–72% yields. UV absorption spectra of the ligands showed four ligand-centered (LC) π–π* transitions and their Ru complexes showed four LC π–π* transitions and one Ru(dπ) → ligand(π*) MLCT. The ligands showed three major emission maxima (λ emission) in the region of 393–418, 416–445, and 437–471 nm in which λ emission is highly dependent on the length of the methylene bridge connecting C3 of benzo[b]-1,10-phenanthroline and C3 of pyridine. Ru complexes with fully aromatic ligand, [Ru(tpy)(4e)]2+, and the most distorted ligand, [Ru(tpy)(4d)]2+, showed two emission maxima at 410 and 444–446 nm, while the others showed one emission at 410 nm. Each of the emission maxima is bathochromatically shifted from the complex with the most distorted ligand (4d) to the complex with fully aromatized planar ligand (4e) indicating lower energy emission. 相似文献
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Crystal Structures of „Supramolecular”︁ Benzo‐18‐crown‐6 Potassium Tetrathiocyanato Metallates: A Dimeric Complex {[K(Benzo‐18‐crown‐6)]2[Hg(SCN)4]}2 and Two Isomeric Complexes [K(Benzo‐18‐crown‐6)][Cd(SCN)3] Containing Trithiocyanato Cadmate Anions with Chain Structures By reaction of potassium thiocyanatomercurate(II) complexes with benzo‐18‐crown‐6 (2,3‐benzo‐1,4,7,10,13,16‐hexaoxacyclooctadec‐2‐ene) crystals of {[K(benzo‐18‐crown‐6)]2[Hg(SCN4)]}2 ( 1 ) were obtained. 1 crystallizes monoclinic, space group P21/n (non‐standard setting of P21/c), a = 1737.35(2), b = 1377.16(2), c = 1984.12(3) pm, β = 100.637(1)°, Z = 2. With potassium tetrathiocyanatocadmate(II) two modifications of a complex [K(benzo‐18‐crown‐6)][Cd(SCN)3] ( 2 , 3 ), of different symmetry were formed. 2 crystallizes monoclinic, P21/c, a = 1158,31(3), b = 1096,55(2), c = 2028,46(2) pm, β = 99,5261(2)°, Z = 4, 3 orthorhombic, P21cn, a = 1105,95(3), b = 1413,07(4), c = 1617,10(5) pm, Z = 4. 1 has a dimeric structure, built up from a dication K2(benzo‐18‐crown‐6)2]2+ and two [K(benzo‐18‐crown‐6)]+ cations, which are bridged by two [Hg(SCN)4]2– anions. In 2 and 3 triply bridged infinite [{Cd(SCN)3–}n] zigzag chains, stretching along screw axes, are to be found as anions. In 2 these chains exist in two conformations related by inversion symmetry, whereas in 3 only one form can be found. [K(benzo‐18‐crown‐6)]+ cations are linked to the anion chains via K · · · S interactions of different lengths. 相似文献
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Peter Gajdoš Soňa Pavlíková Filip Bureš Alžbeta Krutošíková 《Central European Journal of Chemistry》2005,3(2):311-325
The synthesis and reactions of methyl 2-[3-(trifluoromethyl)phenyl]-4H-furo[3,2-b]pyrrole-5-carboxylate (1a) are described. Upon reaction with methyl iodide, benzyl chloride, or acetic anhydride, this compound gave N-substituted products 1b-d. By hydrolysis of compounds 1a-c, the corresponding acids 2a-c were formed, or by reaction with hydrazine-hydrate, the corresponding carbohydrazides 3a-c were formed. By heating 2-[3-(trifluoromethyl)phenly]-4H-furo[3,2-b]pyrrole-5-carboxylic acid (2a) in acetic anhydride, 4-acetyl-2-[3-(trifluoromethyl)phenyl]furo[3,2-b]pyrrole (4) was formed. By hydrolysis of 4, 2-[3-(trifluoromethyl)phenyl]-4H-furo[3,2-b]pyrrole (5a) was formed, and reactions with methyl iodide or benzyl chloride gave N-substituted products 5b-c. The reaction of 4 with dimethyl butynedioate gave substituted benzo[b]furan 6. Compound 3a reacted with triethyl orthoesters giving 7a-c, which afforded with phosphorus (V) sulphide the corresponding thiones 8a-c. The thiones 8a-c reacted with hydrazine hydrate to form hydrazine derivatives 9a-c. The reaction of triethyl orthoformiate with compounds 9a-c led to furo[2′,3′: 4,5]pyrrolo[1,2-d][1,2,4]triazolo[3,4-f][1,2,4]triazines 10a-c. Hydrazones 11a-c were formed from 3a-c and 5-[3-(trifluoromethyl)phenyl]furan-2-carboxaldehyde. The effect of microwave irradiation on some condensation reactions
was compared with “classical” conditions. The results showed that microwave irradiation shortens the reaction time while affording
comparable yields. 相似文献