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1.
以1,6-二氢-6-哒嗪酮-3-甲酰肼(1)与芳香醛反应得到相应的1,6-二氢-6-哒嗪酮-3-羰基芳香醛腙(2a~2e). 再将2a~2e与乙酸酐作用, 合环得到一系列含有1,3,4-噁二唑啉环的衍生物3a~3e; 在DMF中用HSCH2COOH合环, 得到含有4-噻唑烷酮的衍生物4a~4e. 所有化合物的结构均经元素分析, IR, 1H NMR 和MS谱得以证实. 相似文献
2.
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
3.
以苯肼和4-取代苯乙酮(1a~1d)为原料, 经过缩合, 再与Vilsmeier-Haak试剂反应合环, 制得1-苯基-3-芳基-4-甲酰基吡唑(3a~3d), 将其与2-肼基-4/6-取代苯并噻唑(4a~4f)反应, 合成一系列新化合物1-苯基-3-芳基-吡唑-4-醛 [N-(4/6-取代苯并噻唑-2-基)]腙5~8. 所有新化合物的结构均经IR, 1H NMR, MS谱和元素分析证实. 对化合物5~8的荧光进行了测定, 结果显示这些化合物具有荧光特性, 并探讨了化合物的结构对荧光性能的影响. 相似文献
4.
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
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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
8.
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
9.
新型环烷烯并嘧啶并噻唑-3-酮类化合物的合成 总被引:1,自引:0,他引:1
以环戊酮、环庚酮为起始原料合成的环烷烯并[1,2-d]嘧啶-2-硫酮(2)与氯乙酸、芳香醛反应, 合成具有潜在抗癌活性的稠合杂环化合物5-芳基-2,8-二芳亚甲基-2,3,6,7-四氢-5H,8H-环戊烯并[1,2-d]噻唑并[3,2-a]嘧啶-3-酮(3)以及5-芳基-2,10-二芳亚甲基-2,3,6,7,8,9-六氢-5H,10H-环庚烯并[1,2-d]噻唑并[3,2-a]嘧啶-3-酮(4). 3和4的结构经1H NMR, IR, MS分析确认. 相似文献
10.
以豆腐果苷为原料, 在冰醋酸催化下和邻苯二胺缩合生成中间体2-(4-β-D-吡喃阿洛糖苷-苯基)-苯并咪唑(2), 2与卤代烃在K2CO3作用下以乙醇为溶剂合成了一系列1-烃基-2-(4-β-D-吡喃阿洛糖苷-苯基)-苯并咪唑类化合物3a~3h. 新化合物2和3a~3h的结构经1H NMR, IR和MS (HRMS)确认, 并对2和3a~3h进行了药理活性筛选. 结果表明, 部分化合物具有良好的镇静活性; 其中化合物2 (100 mg•kg-1), 3f (100 mg•kg-1)与豆腐果苷相比较具有更强的药理活性. 相似文献
11.
Takehiko Yamato Fenglei Zhang 《Journal of inclusion phenomena and macrocyclic chemistry》2001,39(1-2):55-64
The lower rim functionalizedhexahomotrioxacalix[3]arene triamide derivatives4a and 4b were synthesized from triol 1by a stepwise reaction. Extraction data for alkalimetal ions, transition metal ions, and alkyl ammoniumions from water into dichloromethane are discussed.Due to the strong intramolecular hydrogen bondingbetween the neighboring NH and CO groups, theiraffinities to metal cations were weakened.cone-4a shows a single selectivity ton-BuNH3
plus while partial-cone-4aalmost has no affinity to cations. The anioncomplexation of cone-4a was studied by1H NMR titration experiments. cone-4abinds halides through the intermolecular hydrogenbonding among the NH hydrogens of amide in a 1 : 1fashion in CDCl3. The association constantscalculated from these changes in chemical shifts ofthe amide protons are Ka = 8520 M-1for Cl-1 and Ka = 1720 M-1 forBr-1. cone-4a shows a preference forCl-1 complexation over Br- complexation. Incontrast, cone-4b has good selectivity andaffinity to Agplus cation. A good Job plot proves1:1 coordination of cone-4b withAgplus cation. The complexation mode of cone-4a with n-BuNH3Cl and cone-4b with AgSO3CF3 were also demonstrated by 1H NMR titration in CDCl3. 相似文献
12.
通过3-乙酰基-5-羟甲基异噁唑衍生的Schiff碱2与由醛肟原位生成的腈氧化物的1,3-偶极环加成反应, “一锅法”制备了5-甲基-5-[5-(叔丁基二甲基硅氧基甲基)-3-异噁唑基]-3-芳基-4-(4-甲氧基苯基)-4,5二氢-1,2,4-噁二唑类化合物4a~4e; 同时由3-乙酰基-5-羟甲基异噁唑衍生的α,β-不饱和酮(5)与取代苯肼的环化反应制备了5-(叔丁基二甲基硅氧基甲基)-3-[(1,5-二芳基)-3-(4,5-二氢吡唑基)]-异噁唑类化合物6a~6i. 所有新化合物的结构经核磁共振谱氢谱和碳谱、质谱、红外光谱以及高分辨质谱等进行了确证. 相似文献
13.
Chengcheng Zhao Zheming Ying Xiaojun Tao Mingyue Jiang 《Natural product research》2018,32(13):1548-1553
A new lactam alkaloid named oleraciamide D (1), indentified as (5R)-4-(3-methoxy-4-hydroxyphenyl)-5-(4-hydroxyphenyl)-5,6-dihydropyridin-2(1H)-one, together with five known compounds, indole-3-aldehyde (2), portulacatone (3), N-trans-feruloyloctopamine (4), N-trans-feruloyl-3′-O-methyldopamine (5) and N-trans-feruloyltyramine (6) were isolated from Potulaca oleracea L. Among them, indole-3-aldehyde (2) was isolated from the medicine for the first time. The structure of the new alkaloid was elucidated via UHPLC-ESI-Q-TOF/MS, 1D NMR and 2D NMR. The five known compounds were established by comparing the 1H-NMR and 13C NMR with the reported literature. Oleraciamide D (1) showed cytotoxicity against SH-SY5Y cells when concentration at 50 uM by CCK-8 method. 相似文献
14.
A new pentacyclic triterpenoid fatty acid ester, lupan-20-ol-3(β)-yl hexadecanoate (1), together with lupan-20-ol-3(β)-yl acetate (2), olean-18-en-3(β)-yl hexadecanoate (3), dotriacontanoic acid (4), stigmasterol (5), rubiadin (6), nonadecanoic acid (7), palmitic acid (8) and camptothecin (9) were isolated from the hexane and chloroform extracts of Ophiorrhiza shendurunii from South India. Structures of the isolates were determined by 1H, 13C, 13C DEPT, 1H–1H COSY, HMBC, HSQC, NOESY NMR, FT-IR, DART-MS, ESI-MS, alkaline hydrolysis, derivatisation, GC–MS and HPTLC analyses. O. shendurunii hexane and chloroform extracts showed significant activities against Candida albicans and Fusarium oxysporum. Compounds 1 to 3 showed only moderate antiyeast/antifungal activities. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(7):1076-1085
Planar [Ni(bedtc)(PPh3)Cl] (1), [Ni(bedtc)(PPh3)(NCO)] (2), [Ni(bedtc)(PPh3)(NCS)] (3), [Ni(bedtc)(PPh3)(CN)] (4) and [Ni(bedtc)(dppe)]ClO4 (5) (where bedtc = N-benzyl-N-(2-hydroxyethyl)dithiocarbamate anion, PPh3 = triphenylphosphine and dppe = 1,2-bis((diphenylphosphino)ethane)) were prepared from [Ni(bedtc)2]. Complexes 1–5 were characterized by elemental analysis, electronic, IR and NMR (1H, 13C, and 31P) spectra. Electronic spectra of the complexes show bands corresponding to dz 2 → dxy/dx 2 ? y 2 transitions. The complexes were diamagnetic. IR and 13C NMR studies indicate the mesomeric flow of π-electron density from the dithiocarbamate towards the nickel. In 1H NMR, α-CH2–and β-CH2–protons of–CH2–CH2–OH were equally deshielded. The deshielding for the coordinated phosphorus signals in 31P NMR spectra for all the cases compared with the free phosphine clearly manifests the drift of electron density from the phosphorus toward the metal on complexation. Single crystal X-ray structures of 1–3 indicate that nickel is in a planar environment with short >S2C–N bond distances. In 2, a rare mode of coordination between nickel and cyanate (NCO?) through the nitrogen is observed. Significant asymmetry in Ni–S bond distances were observed for 1–3 clearly supporting the trans influences of Cl?, NCO? and NCS?, respectively, over PPh3. 相似文献
16.
A series of 1,4-disubstituted 1,2,3-triazoles having thioether as well as amide linkage were synthesized from aryl(prop-2-yn-1-yl)sulfanes and 2-azido-N-substituted acetamides through Cu(I) catalyzed click reaction. Structures of newly synthesized compounds (3a–3x) were confirmed by spectral techniques like FTIR, 1H NMR, 13C NMR, and HRMS. The synthesized triazoles were evaluated for in vitro antimicrobial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumoniae, Staphylococcus aureus, Candida albicans, and Aspergillus niger. Compounds 3m and 3q displayed appreciable broad spectrum antimicrobial activity against tested microbial strains. The nanoformulations of compounds 3m and 3q were also prepared and examined against one bacterial strain and one fungal strain. 相似文献
17.
Crenguta Dordea Frédéric Brisach Jaouad Haddaoui Françoise Arnaud-Neu Michael Bolte Alessandro Casnati 《Supramolecular chemistry》2013,25(6):347-357
Calix[4]arene derivatives fixed in the 1,3-alternate conformation and substituted at one side by four carbamoylmethylphosphine oxide (CMPO) residues were synthesised. Two CMPO groups are directly attached to the wide rim, while the second pair is bound to the narrow rim via a tri- or tetramethylene spacer. Similar compounds, in which two CMPO groups at the wide rim are combined with two picolinamide groups or two ionisable carboxylic groups at the narrow rim, were also prepared. Some of these calixarene derivatives were studied as extractants for lanthanides (La3+, Eu3+, Yb3+) and thorium (Th4+) from acidic solution into methylene chloride. For selected samples, stability constants in methanol were determined by spectrophotometric titrations. Three compounds (1b′, 13, 17) in the 1,3-alternate conformation and one intermediate in the cone conformation (18) were confirmed by a crystal structure. 相似文献
18.
Hong-Bo Xu Tong-Hua Yang Pei Xie Shi-Jun Liu Yan-Ni Liang Yu Zhang 《Natural product research》2018,32(9):1088-1094
A new pheophytin, (132S, 17S, 18S)-132-hydroxy-20-chloro-ethylpheophorbide a (3), along with two known analogues (1–2) were isolated from the lichen Usnea diffracta Vainio (Parmeliaceae). Among them, compound 3 was a rare C-20-chloro type pheophytin obtained from lichens. Their structures were elucidated by extensive spectroscopic analysis, and all the compounds were obtained for the first time from U. diffracta. Compounds (1–3) were evaluated for their xanthine oxidase (XO) inhibitory activities in vitro, and the results showed that 1–3 possessed significant enzyme inhibitory actions with IC50 values of 46.9 ± 3.8, 75.9 ± 7.4 and 42.1 ± 1.7 μg/mL, respectively. 相似文献
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《Journal of Coordination Chemistry》2012,65(24):4399-4414
Three 3-amino-1,2,4-triazole (Hatz)-based paramagnetic metal complexes, {[Co2(Hatz)2(nip)2]·H2O}n (1), [Co(atz)(nb)]n (2), and {[Co3(H2O)4(Hatz)6(btc)2]·11.5H2O} (3) (nip2? = 5-nitroisophathalate, nb– = p-nitrobenzolate, and btc3– = 1,2,4-benzenetricarboxylate), were respectively prepared by introducing differently carboxylate-containing rigid coligands. All these complexes were structurally and magnetically characterized by single-crystal and powder X-ray diffractions, elemental analysis, FT-IR spectra, thermogravimetric and magnetic measurements. Complex 1 has a four-connected CdSO4-type framework with binuclear subunits periodically extended by ditopic μ-N1, N3-Hatz and carboxylate-containing linkers. Tetrahedral CoII ions in 2 are periodically interlinked into an undulated layer by anionic μ3-N1,N2,N3-atz? connectors with deprotonated nb– spacers located on the both sides. By contrast, complex 3 is a centrosymmetric trinuclear molecule aggregated by six neutral μ-N1, N3-Hatz molecules. The structural difference of 1–3 is significantly due to the flexible binding modes adopted by triazolyl and carboxylate groups. Additionally, 1 exhibits a field-induced metamagnetic transition from an antiferromagnetic ordering to a weak ferromagnetic state resulting from the magnetic competition between triazolyl and carboxylate mediators. Instead, comparable antiferromagnetic couplings transmitted by cyclic triazolyl groups are observed in the nearest neighbors of 2 and 3. 相似文献
20.
Abstract The N-halosuccinimide glycosylation is a highly selective reaction that leads to trans-configured 1-alkoxy-2-halo-glycosides (halo = bromo, iodo).23 As an exception to the generally observed exclusive formation of α-linked glycosides in such reactions,2 we obtained a 3 / 1 mixture of α- and β-disaccharide 6 and 7, when we treated the silylated glycal 4 with NIS (N-iodosuccinimide) and the glycoside 5.4 The similarly protected arabino glycal 9, on the other hand, gave exclusively the expected α-linked saccharide 11, when treated with NIS and the alcohol component 10.5 Silylated glycals 4 and 9 were obtained from L-digitoxal 1 6 and L-rhamnal 8 7 by treatment with tert-butyldiphenylchlorosilane8 and tert-butyldimethylchlorosilane,9 respectively. In both cases the 3-O-silylated derivatives formed in high yields. Only in case of the ribo-configuration minor amounts of a 4-O-silylated product 3 were identified. 相似文献