共查询到19条相似文献,搜索用时 421 毫秒
1.
2.
3.
4.
5.
6.
以取代苯和丁二酸酐为起始原料, 经Friedel-Crafts反应, 肼合环, Br2/HOAc氧化脱氢后得到一系列1,6-二氢-3-芳基-6-哒嗪酮(2a~2d). 然后将2a~2d与PCl5在POCl3中回流, 得到相应的氯代产物3a~3d, 将其与酰肼作用, 合环后得到一系列未见报道的哒嗪并[3,2-c]1,2,4-三唑类化合物. 所有化合物结构均经元素分析, IR, 1H NMR 和MS谱得以证实, 并对其波谱性质进行了讨论. 相似文献
7.
以1-肼羰亚甲基-2-三氟甲基苯并[d]咪唑(1)为原料, 与芳基异硫氰酸酯在无水乙醇中反应得酰氨基硫脲2a~2d, 继而在氢氧化钠水溶液中合环得4,5-二氢-3-(2-三氟甲基苯并[d]咪唑-1-亚甲基)-4-芳基-1,2,4-三唑-5-硫酮(3a~3d), 然后分别采用超声辐射法和常规加热法与四种胺反应合成了16个未见报道的Mannich碱4a~4d, 5a~5d, 6a~6d和7a~7d. 与常规加热法对比, 超声辐射法具有操作简单, 反应时间短, 条件温和, 产率高, 副反应少等优点, 为此类化合物的合成提供了一种有效的新方法. 目标化合物的结构经元素分析, IR和1H NMR确证. 相似文献
8.
9.
为了寻找高效低毒的非甾体抗炎药物, 将5-氯-2-吲哚酮与氯甲酸苯酯经酯化及水解制得1-苯氧羰基-5-氯-2-吲哚酮, 在4-N,N-二甲氨基吡啶作用下与对甲磺酰基苯甲酰氯反应, 经酸化得1-苯氧羰基-3-[羟基-(p-甲磺酰基)苯甲撑基]-5-氯-2-吲哚酮(II1), 最后与相应的胺(氨)反应, 经盐酸中和制得未见文献报道的目标化合物II2~II15, 其结构经IR, 1H NMR, MS和元素分析确证. 二甲苯致小鼠耳肿胀模型测试显示II10, II11, II15具有明显的抗炎活性; 角叉菜胶致大鼠足跖肿胀模型试验结果表明, II10, II11抗炎活性与双氯芬酸钠和替尼达普钠相当(P>0.05); 其中II11的胃肠道副作用显著小于双氯芬酸钠(P<0.05)和替尼达普钠(P<0.01). 相似文献
10.
熊果酸与氯乙酸乙酯反应制得熊果酸乙氧甲酰基甲酯(2), 2与水合肼反应得到熊果酸甲酰肼甲酯(3), 3与羰基化合物反应得到一系列酰腙4a~4g, 再将4a~4g与乙酸酐作用, 环合得到3-O-乙酰基熊果酸3-乙酰基-2-[(未)取代苯基]-2,3-二氢-1,3,4-噁二唑-5-甲酯(5a~5g). 15个新化合物均未见文献报道, 其结构经1H NMR, IR, MS加以确证, 并进行了药理结果筛选. 结果表明, 部分化合物具有良好的抗炎活性. 其中, 化合物5a (40 mg•kg-1), 5d (40 mg•kg-1), 5g (40 mg•kg-1)与熊果酸相比, 具有更强的疗效. 相似文献
11.
Novel unsymmetrical bissalicylaldimine bis-Schiff bases with a benzo-10-aza-15-crown-5 pendant and their cobalt complexes have been synthesized via condensation of 3 or 5-[(benzo-10-aza-15-crown-5)-10-ylmethyl] salicylaldehyde with the half unit Schiff bases and characterized by ^1H NMR, IR, mass spectroscopy, elemental analysis, molar conductances and molar magnetic susceptibility. 相似文献
12.
Synthesis of Double-Armed Benzo-15-crown-5 and Their Complexation Thermodynamics with Alkali Cations
Yu Liu Jian-Rong Han Zhong-Yu Duan Heng-Yi Zhang 《Journal of inclusion phenomena and macrocyclic chemistry》2005,52(3):229-235
A series of double-armed benzo-15-crown-5 lariats (3–8) have been synthesized by the reaction of 4′, 5′-bis(bromomethyl)-benzo-15-crown-5 (2) with 4-hydroxybenzaldehyde, phenol, 4-chlorophenol, 4-methoxyphenol, 2-hydroxybenzaldehyde, and 4-acetamidophenol in 43 ~ 82% yields, respectively. The complex stability constants (K
S) and thermodynamic parameters for the stoichiometric 1:1 and/or 1:2 complexes of benzo-15-crown-5 1 and double-armed crown ethers 3–8 with alkali cations (Na+, K+, Rb+) have been determined in methanol–water (V/V=8:2) at 25 °C by means of microcalorimetric titrations. As compared with the parent benzo-15-crown-5 1, double-armed crown ethers 3–8 show unremarkable changes in the complex stability constants upon complexation with Na+, but present significantly enhanced binding ability toward cations larger than the crown cavity by the secondly sandwich complexation. Thermodynamically, the sandwich complexations of crown ethers 3-8 with cations are mostly enthalpy-driven processes accompanied with a moderate entropy loss. The binding ability and selectivity of cations by the double-armed crown ethers are discussed from the viewpoints of the electron density, additional binding site, softness, spatial arrangement, and especially the cooperative binding of two crown ether molecules toward one metal ion. 相似文献
13.
Synthesis of Double-Armed Benzo-15-crown-5 and Their Complexation Thermodynamics with Alkali Cations
A series of double-armed benzo-15-crown-5 lariats (3–8) have been synthesized by the reaction of 4′, 5′-bis(bromomethyl)-benzo-15-crown-5 (2) with 4-hydroxybenzaldehyde, phenol, 4-chlorophenol, 4-methoxyphenol, 2-hydroxybenzaldehyde, and 4-acetamidophenol in 43 ~ 82% yields, respectively. The complex stability constants (K
S) and thermodynamic parameters for the stoichiometric 1:1 and/or 1:2 complexes of benzo-15-crown-5 1 and double-armed crown ethers 3–8 with alkali cations (Na+, K+, Rb+) have been determined in methanol–water (V/V=8:2) at 25 °C by means of microcalorimetric titrations. As compared with the parent benzo-15-crown-5 1, double-armed crown ethers 3–8 show unremarkable changes in the complex stability constants upon complexation with Na+, but present significantly enhanced binding ability toward cations larger than the crown cavity by the secondly sandwich complexation. Thermodynamically, the sandwich complexations of crown ethers 3-8 with cations are mostly enthalpy-driven processes accompanied with a moderate entropy loss. The binding ability and selectivity of cations by the double-armed crown ethers are discussed from the viewpoints of the electron density, additional binding site, softness, spatial arrangement, and especially the cooperative binding of two crown ether molecules toward one metal ion.Graphical Abstract Synthesis of Double-Armed Benzo-15-crown-5 and Their Complexation Thermodynamics with Alkali CationsYU LIU*, JIAN-RONG HAN, ZHONG-YU DUAN and HENG-YI ZHANG
This revised version was published online in July 2005 with a corrected issue number. 相似文献
14.
Özlem Sarıöz Osman Serindaĝ Meysun İ. Abdullah 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):1785-1795
Functionalized bis(amino)phosphines of the type PhP(NHR)2 ( 1a–c ) and aminophosphines of the type Ph2PNHR ( 2a–c ) have been synthesized by treating PhPCl2 or Ph2PCl with corresponding primary amines of H2N-R where R = -CH2SO3H, -C6H4SO3H, and benzo-15-crown-5. The molybdenum(0) complex of the aminophosphine ( 3 ) has been obtained by reacting cis-[Mo(CO)4(bipy)] with aminophosphine ( 2c ). The synthesized aminophosphines, bis(amino)phosphines, and the molybdenum(0) complex have been characterized by IR, 1H NMR, 31P NMR, and MS spectroscopic techniques and by elemental analysis. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(2):139-149
Abstract 7Lithium NMR measurements were used to determine the stoichiometry and stability of Li+ complexes with 12-crown-4, 15-crown-5 and benzo-15-crown-5 in acetonitrile solution. A competitive 7Li NMR technique was also employed to probe the complexation of Mg2+, Ca2+, Co2+, Ni2+, Cu2+, Zn2+ and Cd2+ ions with the same crown ethers. In all cases, the stability of the resulting 1:1 complexes was found to decrease in the order 15-crown-5 > benzo-15-crown-5 > 12-crown-4. Ca2+ and Cd2+ ions formed the most stable complexes in the series. 相似文献
16.
Reductive amination of 4′-formyl[benzo-15-crown-5] with sodium cyanoborohydride in the NH4Ac/MeOH medium followed by acid addition and extraction with CHCl3 unexpectedly lead to the isolation of the salt (B15C5-CH2-NH3)+-(H3BCNBH2CN)− with an unusual dicyanodiborohydride anion. The self-complementary 4′-ammoniomethyl[benzo-15-crown-5] cation was found to exist as a supramolecular dimer in the solid state, acetonitrile solution, and gas phase as revealed by X-ray crystallography, NMR and mass spectrometry, respectively. 相似文献
17.
Two new ditopic receptors for α,ω-alkanediyldiammonium cations based on a tetraazamacrocyclic (cyclidene) nickel(II) complex bearing two crown-ether residues were synthesized. The studies of the host-guest interaction between the receptors and a series of α,ω-diammonium salts by NMR titration in acetonitrile-d3 showed that 1:1 complexes are formed with Kassoc∼103-105 M−1. Receptor 1 with benzo-15-crown-5 arms showed substantial selectivity in binding of trimethylene- and tetramethylenediammonium dications, and 1-2 orders of magnitude weaker binding of shorter (C2) or longer (C5 and C6) diammonium cations. Receptor 2 with benzo-18-crown-6 arms showed higher affinity to all studied diammonium cations, but the recognition of the length of α,ω-diammonium cations was less pronounced. 相似文献
18.
Christelle Mouveaux Joëlle Levalois-Mitjaville Roger De Jaeger 《Journal of inclusion phenomena and macrocyclic chemistry》2001,39(3-4):253-259
The complexation behaviour between salts of Li+-Rb+ in CD3CN and tris(benzocrown ether)s 2a,bX=P(NMeN=CH-B15C5)3 (X = O, S) and tri[bis(benzocrown ether)][N=P(NMeN=CH-B15C5)2]3
3 was investigated by 13 C NMR spectroscopy. Using the program RMNSTAB, the complexation constants for the different possible complexes (M2L, ML andML2 were L represents one benzo-15-crown-5) were obtained and were compared with those of the corresponding monomer material. A remarkable ``biscrown effect' for compounds 2a,b and 3 was found, especially for potassium and rubidium by the predominant formation of stable ML2 complexes. The strong chelate effect make these ligands highly efficient extracting agents for alkali metal picrate salts of K+, Rb+ and Cs+,as shown by UV-Vis spectroscopy. 相似文献
19.
Two novel supramolecular aggregations possessing column structures have been prepared from double-armed benzo-15-crown-5 ether (2) and its complex with potassium ion, respectively. Their molecular assembly behavior has been evaluated by calorimetry, 1H NMR, X-ray crystallography and STM images, revealing that the molecular assembly behavior of 2 in the solid state can be controlled by the stepwise sandwiching complexation with the cation. 相似文献