一步法合成噻唑并[3,2-b](1,2,4)-三唑类衍生物的研究

以3-芳基-5-巯基-1,2,4-三唑为原料, 在酸性条件下与乙酰丙酮和乙酰乙酸乙酯一步成环, 制备得到12种新的2-芳基-5-取代-6-甲基噻唑并[3,2-b](1,2,4)-三唑类衍生物. 所有化合物结构经IR, 1H NMR, 13C NMR 和MS及元素分析确证.     

3-乙基苯并噻唑螺萘并噁嗪与牛血清白蛋白的相互作用

采用荧光光谱法和热力学方法研究了3-乙基苯并噻唑螺萘并噁嗪(EBSN)与牛血清白蛋白(BSA)的相互作用.结果表明,在pH为7.46的Tris-HCl及0.01mol·L-1的NaCl介质中,EBSN能强烈猝灭BSA的荧光,猝灭机理为形成复合物的静态猝灭.在298、306和313K时,两者的表观结合常数Kb分别为1.762 0×104,3.396 3×104和6.123 5×104 L·mol-1.与此同时,EBSN与BSA的结合反应是自发的,作用力主要为疏水作用力;BSA和EBSN的工作曲线分别为F0-F=2.439c-8.322和(F0-F)/F=0.061 89c+0.556 6,对BSA和EBSN的检出限分别为0.015mg·L-1和7.61×10-7 mol·L-1.     

新型环烷烯并嘧啶并噻唑-3-酮类化合物的合成

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.     

噻唑并嘧啶类化合物的合成研究进展

综述了在医药和农药领域具有广泛用途的噻唑并嘧啶类化合物近二十年来合成方法上的研究进展. 结合本研究组在这一领域的工作介绍了噻唑并嘧啶类化合物的三种主要结构类型: 噻唑并[3,2-a]嘧啶、噻唑并[4,5-d]嘧啶、噻唑并[5,4-d]嘧啶类化合物的相关合成方法及新进展.     

咪唑并吡啶化合物的合成研究进展

咪唑并吡啶类化合物是一类非常重要的含氮稠杂环化合物, 在医药、农药和染料工业有着广泛的应用. 该类化合物由于其特定的生理活性以及和吲哚、氮杂吲哚等在结构上的类似性, 引起了人们广泛的兴趣. 常见的咪唑并吡啶类化合物有咪唑并[1,2-a]吡啶、咪唑并[1,5-a]吡啶、咪唑并[4,5-b]吡啶和咪唑并[4,5-c]吡啶等类型. 以咪唑并[1,2-a]吡啶和咪唑并[1,5-a]吡啶化合物为例, 阐述该类化合物近十年来的合成研究进展.     

2-(p-氯苯)-5,8-二氢螺咪唑并〔2,1-b〕苯并〔d〕噻唑7(6H),1′-环己烷的合成及晶体结构

合成了2－（p-氯苯）-5，8-二氢螺咪唑并[2，1-b]苯并[d]噻唑7（6H），1’-环乙烷5，并测定了其晶体结构。晶体分子式晶体属单科晶系，空间群为结构的偏离因子分子结构中有一个大的平面部分，是由噻唑五员环（A）和咪唑五员环（B）构成。     

6-硝基苯并咪唑杂环衍生物的合成

以６－硝基苯并咪唑－１－乙酰肼和５－（６－硝基苯并咪唑－１－亚甲基）－３－巯基－４－氨基－１,２,４－三唑为原料,在不同条件下合成了一系列新的均三唑〔３,４－ｂ〕－１,３,４－噻二唑,１,２,４－三唑和１,３,４－恶二唑衍生物。化合物的结构均经元素分析、＾１Ｈ ＮＭＲ、ＩＲ和ＭＳ确证,并对其波谱性质进行了讨论。     

苯并异噻唑啉酮类化合物的合成与活性研究

通过烷基醇与固体三光气(BTC)反应后加入1,2-苯并异噻唑啉-2(3H)-酮(BIT)继续反应的“一锅法”制备了8种未见文献报道的2-(苯并异噻唑啉-3-酮-2-基)甲酸酯类化合物.化合物结构经IR、1HNMR和元素分析确认,并且对枯草芽孢杆菌、金黄色葡萄球菌、嗜水单细胞菌和大肠杆菌进行了初步抑菌活性实验,实验结果表...     

Synthesis of Novel Spiro Pyrrolidine and Pyrrolizine Derivatives by 1,3-Dipolar Cycloaddition

The 1,3‐dipolar cycloaddition of azomethine ylides derived from isatin and amino acids viz. sarcosine and proline to 2‐arylmethylidene‐5,6‐dihydroimidazo[2,1‐b]thiazol‐3(2H)‐ones afforded novel spiro pyrrolidines and pyrrolizidines regio‐ and stereoselectively in moderate yields. The products were characterized thoroughly by IR, MS, NMR together with elementary analysis.     

六(乙氧基吡咯烷酮)三聚磷腈的合成与表征

以N-羟乙基吡咯烷酮与氢化钠作用生成相应的钠盐,再将此钠盐与六氯三聚磷腈(HCCP)发生亲核取代反应,合成了六(乙氧基吡咯烷酮)三聚磷腈,用IR、31P NMR、1H NMR、13C NMR、DEPT、FABMS等现代谱学技术对其结构进行了表征。生物活性试验表明,此化合物1mg/mL时对腐生线虫Panagrellus redivivus的72h致死率为52·7%。     

A New Four‐Component Reaction for the Synthesis of Spiro[4H‐indeno[1,2‐b]pyridine‐4,3′‐[3H]indoles]

A new four‐component synthesis of spiro[4H‐indeno[1,2‐b]pyridine‐4,3′‐[3H]indoles] and spiro[acenaphthylene‐1(2H),4′‐[4H‐indeno[1,2‐b]pyridines] by the reaction of indane‐1,3‐dione, 1,3‐dicarbonyl compounds, isatins (=1H‐indole‐2,3‐diones) or acenaphthylene‐1,2‐dione, and AcONH₄ in refluxing toluene in the presence of a catalytic amount of pyridine is reported.     

Separation and Thermal Racemization of the Enantiomers of Spiro[cyclohexadiene-dihydroacridines]

Summary.  The enantiomers of substituted spiro[cyclohexadiene-dihydroacridines] were separated by enantioselective liquid chromatography with the sorbent/solvent systems triacetylcellulose/methanol, tris-(3,5-dimethylphenylcarbamoyl)-cellulose/silica gel (Chiralcel OD^TM)/n-heptane/2-propanol, and (+)-poly-(trityl methacrylate)/silica gel/n-heptane/2-propanol. Interconversion barriers of the enantiomers were determined for a series of derivatives by thermal racemization. Electrocyclic ring opening/ring closure in terms of the Woodward-Hoffmann rules is discussed for the enantiomerization mechanism; the interconversion of the enantiomers by enolization is ruled out by deuterium exchange experiments. Received April 3, 2000. Accepted April 12, 2000     

Investigation of the Reactions of Indole‐2,3‐diones with Biuret: A Novel Approach for the Synthesis of Spiro[indole‐triazines]

Reactions of indole‐2,3‐diones with biuret afforded 1,3‐dihydro‐3‐ureidoformimido‐2H‐indol‐2‐ones and spiro[3H‐indole‐3,2′(1′H )‐(1,3,5)triazine]‐2,4′,6′(1H ,3′H ,5′H )‐triones indicated these to be solvent dependent. The chemical structures of the products were elucidated by their comprehensive spectroscopic (IR, ¹H‐NMR, ¹³C‐NMR, ¹⁹F‐NMR, and Mass) as well as analytical analysis.     

Facile synthesis and characterization of novel benzo-fused macrocyclic dicarbonitriles and pyrazolo-fused macrocycles containing thiazole subunits

Abstract

Novel bis[2-(thiazol-2-yl)acetonitriles], linked to aliphatic cores via ethers, were prepared by the reaction of the appropriate bis(2-bromoethan-1-one) with 2-cyanothioacetamide in dioxane at reflux. Bis[2-(thiazol-2-yl)acetonitriles] were taken as key intermediates for the preparation of a new class of macrocyclic dicarbonitriles bearing two thiazole units and containing two O₂-donor sets and fused with two benzene units. The target macrocyclic dicarbonitriles were prepared by the cyclocondensation of bis[2-(thiazol-2-yl)acetonitriles] with the appropriate bis(aldehydes) in N,N-dimethylformamide in the presence of piperidine at reflux. Moreover, a new class of pyrazolo-fused macrocycles containing thiazole subunits were prepared by the reaction of macrocyclic dicarbonitriles with hydrazine hydrate in ethanol at reflux. The structures of the novel macrocycles bearing thiazole subunits were elucidated by considering their elemental analyses as well as their IR, mass, ¹H NMR and ¹³C NMR spectral data.     

Synthesis and Crystal Structure of Dicesium trans Dicarbonatotetraaquomagnesium, Cs_2[Mg(CO_3)_2(H_2O)_4]

ＩｎｔｒｏｄｕｃｔｉｏｎＰｒｅｖｉｏｕｓｌｙ,ｗｅｒｅｐｏｒｔｅｄｔｈｅｃｒｙｓｔａｌｓｔｒｕｃｔｕｒｅｏｆＫ２［Ｎｉ（ＣＯ３）２（Ｈ２Ｏ）４］［１］,ｗｈｉｃｈｃｒｙｓｔａｌｌｉｚｅｄｉｎｔｈｅｂａｙｌｉｓｓｉｔｅｔｙｐｅｓｔｒｕｃｔｕｒｅａｎｄｗａｓｆｏｕｎｄｔｏｂｅｉｓｏｓｔｒｕｃｔｕｒａｌｗｉｔｈＫ２［Ｃｏ（ＣＯ３）２（Ｈ２Ｏ）４］［２］ａｎｄＫ２Ｍｇ（ＣＯ３）２·４Ｈ２Ｏ［３］．Ｉｎｏｒｄｅｒｔｏｓｙｓｔｅｍａｔｉｃａｌｌｙｉｎｖｅｓｔｉｇａｔｅｔｈｅｏｃｃｕｒｒｅｎｃｅｏｆｔｈｅｃｏ…     

4—取代苯基—6—甲基—5—硫代—1,2,4—三嗪—3—酮的合成

合成了一系列新的４，６－二取代－５－硫代－１，２，４－三嗪－３－酮类化合物，并用元素分析、ＩＲ、＾１Ｈ ＮＭＲ及ＭＳ对其结构进行了表征。     

羰基钴及其盐的合成方法研究进展

详细评述了羰基钴及其盐的合成方法。参考文献４５篇。