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利用生物活性叠加原理,将"邻羟苯基"和"咪唑烷"分子片断有机结合,以水杨醛和乙二胺为起始原料,经缩合、NaBH4还原制得N,N'-二邻羟苄基乙二胺(2),进而与芳醛类化合物缩合关环,合成了8种N,N'-二(2-羟苄基)取代咪唑烷类化合物(3a~3h). 化合物的结构经1H NMR、IR、MS和元素分析等测试技术进行了表征. 结果表明,水杨醛与乙二胺的缩合反应,可专一性地生成对称双缩席夫碱化合物(1);芳醛上的取代基对缩合关环反应有显著影响,邻、对位吸电基可使芳醛的羰基活化,有利于缩合关环反应的进行,邻、对位供电基可使芳醛的羰基钝化,不利于缩合关环反应进行. 抑菌测试结果表明,质量分数为0.1%时,N,N'-二(2-羟苄基)取代咪唑烷化合物对不同菌株的抑菌活性具有明显的特异性,对白色念珠菌、大肠杆菌的抑菌率达100%. 相似文献
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水合茚三酮与芳甲基酮、水合肼缩合环化制得2-芳基-3,4-二氮杂芴酮(2); 2经还原得2-芳基-3,4-二氮杂芴(3).2与2-溴联苯格氏试剂反应得到中间体叔醇(4); 4在酸性条件下关环合成了2-芳基-3,4-二氮杂螺二芴,其结构经1H NMR,13C NMR和元素分析表征. 相似文献
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合成了新型1,7-双(N-取代氨基甲基)-2,8-二羟基-朝格尔碱(4),以4为催化剂催化了4-羟基香豆素和2-亚苄基丙二腈[或甲基(乙基)-2-氰基-3-苯基丙烯酸]的Aldol反应,获得了一系列化合物8;以4为配体与钯联合催化了串联Aldol-Ullmann反应,得到了化合物10和12.测试了所有化合物对人三阳性乳腺癌细胞(MCF-7)、人三阴性乳腺癌细胞(MDA-MB-231)、人肝癌细胞(HepG2)和人肝癌细胞(MHCC-97H)的抗癌活性以及对人肝细胞(LO2)的细胞毒性.其中,1,7-双((甲基氨基)甲基)-6H,12H-5,11-甲二苯并[b,f][1,5]二氮芳辛-2,8-二醇(4b)对MCF-7(抑制率>30%)、1,7-双((((1-苯乙基)氨基)甲基)-6H,12H-5,11-甲二苯并[b,f][1,5]二氮芳辛-2,8-二醇(4d)和1,7-双(((吡啶-2-基甲基)氨基)甲基)-6H,12H-5,11-甲基二苯并[b,f][1,5]重氮-2,8-二醇(4e)对MDA-MB-231具有较高的选择性和抑制活性, 2-氨基-5-氧代-4-(3,4,5-三甲氧... 相似文献
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在邻羟基偶氮化合物的吡啶环上引入卤素原子,可以提高试剂的灵敏度和颜色对比度,但一般认为以引入一个卤素原子为好。另外,在芳环偶氮基的对位上引入较强的推电子官能团也有助于提高试剂的灵敏度。目前用的3,5-二溴-PEDAP就是根据上述原则合成的一种双卤素取代邻羟基偶氮试剂。我们用甲基代替乙基,合成了2-(3,5-二溴-2-吡啶偶氮)-5-二甲氨基酚[3,5-Br2-DMPAP],并考察了它的基本性质和用作分析试剂的可能性。实验表明:在适当条件下,它可同很多阳离子发生颜色反 相似文献
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Compounds [Rb(18-crown-6)]4As14.6NH3 (1) and [Li(NH3)4]4P14.NH3 (2) were prepared by the reaction of Rb4As6 with SbPh3 and 18-crown-6 and by the reduction of white phosphorus with elemental lithium in liquid ammonia, respectively. Both were characterized by low-temperature single-crystal X-ray structure analysis. They were found to contain the Ci symmetrical Pn14(4-) anion (Pn = P, As), which consists of two nortricyclane-like Pn7-cages connected by a single bond. Molecular complexes of [Rb(18-crown-6)(NH3)]2[Rb(18-crown-6)]2As14 are formed in 1, which are connected to fanfold sheets via N-H...O bonds. The anion is isolated in 2, and N-H...N bonds result in the formation of {[Li(NH3)4](mu-NH3)2[Li(NH3)4]}2+ cationic complexes. 相似文献
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二茂铁硫冠醚的合成和性质的研究,近年来 Sato 等做了不少工作,其化合物的主要类型如下: 相似文献
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以4,4′-(α,ω-辛二酰氧)二苯甲酰氯(M1)、2,5-二(对十二烷氧基苯甲酰氧基)对苯二酚(M2)和顺式-4,4′-双(4-羟基苯基偶氮)二苯并-14-冠-4(M3)为单体,通过溶液共缩聚反应,合成了一系列含X-型二维液晶基元和顺式-4,4′-双(4-羟基苯基偶氮)二苯并-14-冠-4冠醚环的主链型液晶共聚酯.单体1(M1)由对羟基苯甲酸和辛二酰氯,通过酯化和取代反应制备,单体2(M2)由2,5-二羟基苯醌和对十二烷氧基苯甲酰氯通过酯化和还原反应制备,单体3(M3)由顺式-二氨基二苯并-14-冠-4和苯酚通过重氮化和偶联反应制备.共聚酯的分子量不高,[η]在0·35~0·25dL/g之间.单体的化学结构通过IR、UV、1H-NMR、MS和元素分析等方法确证.共聚酯的外观为黄色粉状固体,除CP9外,室温下不溶于CHCl3和THF溶剂.共聚酯的性质采用GPC、[η]、DSC、TG、WAXD和POM等方法进行了研究.发现所有的共聚酯加热到各自的熔融温度以上都能形成液晶态,在液晶态可以观察到向列相的丝状织构或纹影织构.共聚酯的熔融温度(Tm)和各向同性温度(Ti)随共聚酯分子中顺式-4,4′-双(4-羟基苯基偶氮)二苯并-14-冠-4用量的改变呈规律性变化.WAXD研究进一步证实了共聚酯的液晶性. 相似文献
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A new series of 4-substituted derivatives of dibenzo-14-crown-4 including 4-nitro-DB14-crown-4 ( 2a ), 4-bromo-DB14-crown-4 ( 2b ), 4-chloro-DB14-crown-4 ( 2c ) and 4-formyl-DB14-crown-4 ( 2d ) has been synthesized with and without a lithium cation template. No matter with or without the template, a satisfactory correlation between the nature of the substituent group on the benzene ring and the reaction yield is observed. The larger σ values for the substituent groups gave lower yields. 相似文献
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Takayo Moriuchi-Kawakami Rie Aoki Kazuhiro Morita Haruhisa Tsujioka Keiichi Fujimori Yasuhiko Shibutani Toshiyuki Shono 《Analytica chimica acta》2003,480(2):291-298
A conformational analysis was performed on two crown ethers (12-crown-3 and 12-crown-4) using a combination of semi-empirical and ab initio methods. The lowest conformations of 12-crown-3 and 12-crown-4 were found to have exodentate C3v and C2 structure, respectively. In the case of the sandwich-type complexation, the nucleophilic cavity of 12-crown-3 rather than that of 12-crown-4 seemed to be optimal for complexation with the Na+ ion. Four new bis(12-crown-3) derivatives (1–4) were examined as potential sodium ion-selective ionophores in poly(vinylchloride) (PVC) membrane electrodes. The ion-selective electrode (ISE) based on di(1,5,9-trioxacyclododecanylmethyl) 2-dodecyl-2-methylmalonate (1) had the highest selectivity for the sodium ion among the alkali and alkaline earths studied. The sodium ion selectivity of the ISE based on bis(12-crown-3) derivative 1 was superior to that of the ISE based on the bis(12-crown-4) analogue. 相似文献
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Habata Y Seo J Otawa S Osaka F Noto K Sung Lee S 《Dalton transactions (Cambridge, England : 2003)》2006,(18):2202-2206
Diazahexathia-24-crown-8 (2) has been isolated from the reaction mixture during the preparation of monoazatrithia-12-crown-4 (1). When N-Boc protected bis(2-chloroethyl)amine was employed as a starting material, N-Boc protected monoazatrithia-12-crown-4 (3) and N-Boc protected diazahexathia-24-crown-4 (4) were separated easily. Double-armed diazahexathia-24-crown-8 having two 3',5'-dichlorobenzyl groups (5a) or two 2-phenylethyl groups (5b) were also prepared using reductive amination. The stoichiometry and detailed structures of the Ag+ complexes with and were investigated by 1H NMR titration experiments and X-ray crystallography. 相似文献
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By anaerobic incubation of pinoresinol diglucoside (1) from the bark of Eucommia ulmoides with a fecal suspension of humans, eleven metabolites were formed, and their structures were identified as (+)-pinoresinol (2), (+)-lariciresinol (3), 3'-demethyl-(+)-lariciresinol (4), (-)-secoisolariciresinol (5), (-)-3-(3", 4"-dihydroxybenzyl)-2-(4'-hydroxy-3'-methoxybenzyl)butane-1, 4-diol (6), 2-(3', 4'-dihydroxybenzyl)-3-(3", 4"-dihydroxybenzyl)butane-1, 4-diol (7), 3-(3"-hydroxybenzyl)-2-(4'-hydroxy-3'-methoxybenzyl)butane-1, 4-diol (8), 2-(3', 4'-dihydroxybenzyl)-3-(3"-hydroxybenzyl)butane-1, 4-diol (9), (-)-enterodiol (10), (-)-(2R, 3R)-3-(3", 4"-dihydroxybenzyl)-2-(4'-hydroxy-3'-methoxybenzyl)butyrolactone (11), (-)-(2R, 3R)-2-(3', 4'-dihydroxybenzyl)-3-(3", 4"-dihydroxybenzyl)butyrolactone (12), (-)-(2R, 3R)-3-(3"-hydroxybenzyl)-2-(4'-hydroxy-3'-methoxybenzyl)butyrolactone (13), 2-(3', 4'-dihydroxybenzyl)-3-(3"-hydroxybenzyl)butyrolactone (14), 2-(3'-hydroxybenzyl)-3-(3", 4"-dihydroxybenzyl)butyrolactone (15) and (-)-(2R, 3R)-enterolactone (16) by various spectroscopic means, including two dimensional (2D)-NMR, mass spectrometry and circular dichroism. A possible metabolic pathway was proposed on the basis of their structures and time course experiments monitored by thin-layer chromatography. Furthermore, a bacterial strain responsible for the transformation of (+)-pinoresinol to (+)-lariciresinol was isolated from a human fecal suspension and identified as Enterococcus faecalis strain PDG-1. 相似文献
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Abstract Competitive transport of alkali and alkaline earth cations has been carried out by using a mixed carrier system composed of dibenzo-14-crown-4 and bis(2-ethylhexyl)phosphoric acid. In the absence of crown ether, bis(2-ethylhexyl)phosphoric acid transported alkaline earth cations with high selectivity. The combination of dibenzo-14-crown-4 and bis(2-ethylhexyl)phosphoric acid showed a synergistic enhancement in lithium transport, and the enhancement effect was not apparent in transport of other cations. On the other hand, the mixed carrier systems consisting of dibenzo-14-crown-4 and dodecylbenzenesulfonic acid, and of dibenzo-14-crown-4 and 1-bromohexadecanoic acid exhibited the enhancement effects both in lithium transport and in sodium transport. The formation of the synergistic complex was analyzed by using fast atom bombardment mass spectrometry. 相似文献
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van Nostrum CF Benneker FB Brussaard H Kooijman H Veldman N Spek AL Schoonman J Feiters MC Nolte RJ 《Inorganic chemistry》1996,35(4):959-969
The synthesis of novel magnesium, copper, and metal-free porphyrazines, peripherally substituted with dithia-7-crown-2 (MPz(7)), dithia-15-crown-5 (MPz(15)), and dithia-18-crown-6 (MPz(18)) macrocycles is reported. These compounds are prepared starting from dicyanoethylene containing crown ethers 3, 2(1), and 2(2), respectively, which contain sulfur as well as oxygen heteroatoms. The "crowned" porphyrazines bind silver(I) and mercury(II) perchlorates. UV/vis spectroscopy and electron paramagnetic resonance measurements reveal that addition of the transition-metal ions leads to dimerization of the porphyrazine complexes. In the case of the dithia-18-crown-6-substituted porphyrazines, the dimers break up to form monomeric 6:1 guest-host complexes when more than 2 equiv of the metal ion is added. The single-crystal structures of the crown ether 2(2) and the porphyrazine MgPz(18) are presented. Compound C(14)H(20)N(2)O(4)S(2) (2(2)) crystallizes in the monoclinic space group P2(1)/c with a = 10.9310(13) ?, b = 19.383(3) ?, c = 8.6976(14) ?, beta = 108.898(11) degrees, V = 1743.5(5) ?(3), and Z = 4. The structure refinement converged to R = 0.0366 and R(w) = 0.0504. Compound C(56)H(82)MgN(8)O(17)S(8) (MgPz(18)) crystallizes in the triclinic space group P&onemacr; with a = 9.584(3) ?, b = 17.672(2) ?, c = 19.620(4) ?, alpha = 84.904(14) degrees, beta = 85.21(2) degrees, gamma = 89.29(2) degrees, V = 3298.4(13) ?(3), and Z = 2. The structure refinement converged to R1 = 0.0839 and wR2 = 0.2196. The electrical properties of H(2)Pz(18) have been studied by complex impedance spectroscopy. The bulk electrical conductivity of this compound is approximately 1 order of magnitude higher than that of the corresponding 18-crown-6 phthalocyanine. 相似文献