新型N-（4，6-双取代嘧啶-2-基）-N’-（三氟甲基苯基）胍的合成，结构及生物活性研究

设计,合成了10种新型的胍衍生物,结构经FTIR, MS, 1H NMR 和元素分析确证,并且采用X-射线衍射分析方法确证了具有较好生物活性的化合物11a的结构。并且对这些化合物进行了除草活性测试,结果表明化合物11a,11b,11c在100µg·mL-1 对油菜具有较好的抑制作用,初步的KARI活性结果表明这些化合物对KARI的活性很弱。     

芳基吡唑氟尿嘧啶类化合物的设计、合成与杀虫活性研究

利用以γ-氨基丁酸(GABA)受体抑制剂芳基吡唑类杀虫剂的关键结构5-氨基-3-氰基-1-(取代苯基)吡唑为基本母核,设计、合成了26个创新结构芳基吡唑氟尿嘧啶化合物.目标化合物结构均采用1H NMR,FTIR和元素分析进行了结构确证,以小菜蛾和库蚊为靶标进行了杀虫活性测试.评价结果表明创制化合物具有优越的杀虫活性:在浓度为1000 mg·L-1时,化合物5a~5c,5e,5m及5u对库蚊具有100%的杀虫活性;在浓度为400 mg·L-1时,化合物5p对小菜蛾具有94.5%的杀虫活性.初步构效关系研究表明:苯环上取代基种类及位置等对化合物的生物活性有重要的影响.     

蘑菇组织催化氧化-流动注射荧光法测定去甲肾上腺素和左旋多巴

研究发现富含多酚氧化酶的蘑菇组织可催化溶解氧氧化去甲肾上腺素和左旋多巴在碱性条件下生成具有强荧光的三羟基和二羟基吲哚类物质 ,建立了以蘑菇组织柱为酶反应器的去甲肾上腺素和左旋多巴的流通式荧光分析法 .该法对去甲肾上腺素和左旋多巴响应的线性范围分别为 6× 10 -8～ 1× 10 -5g·mL-1和 3× 10 -8～ 1× 10 -5g·mL-1,检测限分别为 2×10 -8g·mL-1和 1× 10 -8g·mL-1( 3S/k) .该组织反应器可连续使用 14d ,对 1× 10 -7g·mL-1去甲肾上腺素和 1× 10 -7g·mL-1左旋多巴测定的相对标准偏差 (R .S .D .)均小于 3 % (n =11) .详细研究了常见离子和抗氧化剂对本体系的干扰情况 .将该体系用于药物制剂中去甲肾上腺素和左旋多巴含量的测定 ,结果与药典标准方法测得值一致 .实验结果证明了方法的可行性和可靠性     

2-氧代-2-[1-(3-吡啶甲基氨基)-1''''-芳基]甲基-4-芳基-5,5-二甲基-1,3,2-二氧磷杂环己烷的合成与生物活性

采用环状亚磷酸酯与亚胺的加成反应, 合成了9个未见文献报道的含吡啶基的α-氨基环状膦酸酯化合物. 其结构经1H NMR, 31P NMR, MS 和元素分析确证, 同时采用X射线单晶衍射对化合物3i的立体构型进行了进一步确证. 测定了该系列化合物的杀虫、杀菌和除草活性, 结果表明, 化合物的杀虫活性虽然较差, 但所有化合物在药液质量浓度为1.0×10-4 g/mL时都具有较好的除草活性, 部分化合物在5.0×10-5 g/mL时显示出良好的杀菌活性.     

2-胺基(芳氧基)-5,8,9-三甲基噻吩并吡啶并[4,3-d]嘧啶-4(3H)-酮的合成和生物活性

利用串联Aza-Wittig法合成了两类共计16个未见文献报道的噻吩并吡啶并嘧啶类化合物, 通过IR, ¹H NMR, EI-MS, 元素分析等方法对所合成的化合物进行了结构表征, 化合物II-1还通过了X单晶衍射的进一步确证. 并初步测定了所合成化合物的杀虫、杀菌和除草活性. 结果表明: 所测化合物的杀虫活性较差, 但大部分化合物具有一定的除草活性和良好的杀菌活性.     

Aspernigerin类似物的合成及生物活性研究

以天然产物Aspernigerin为先导,将Aspernigerin结构中的一个1,2,3,4-四氢喹啉基团以芳胺类化合物替代,设计合成了15个未见文献报道的Aspernigerin类似物,结构均经过1H NMR,IR和元素分析确证.初步生物活性测试表明,大部分目标化合物均表现出了一定的杀虫和杀菌活性,其中化合物2n在200μg/mL的浓度下对小菜蛾仍表现出100%的杀虫活性,优于先导Aspernigerin和对照药剂噻虫嗪;化合物2d,2e,2j,2k表现出对黄瓜灰霉病优于先导Aspernigerin的抑制活性.     

2-氧代-2-[1-(3-吡啶甲基氨基)-1′-芳基]甲基-4-芳基-5,5-二甲基-1,3,2-二氧磷杂环己烷的合成与生物活性

采用环状亚磷酸酯与亚胺的加成反应,合成了9个未见文献报道的含吡啶基的α-氨基环状膦酸酯化合物.其结构经1H NMR,31P NMR,MS和元素分析确证,同时采用X射线单晶衍射对化合物3i的立体构型进行了进一步确证.测定了该系列化合物的杀虫、杀菌和除草活性,结果表明,化合物的杀虫活性虽然较差,但所有化合物在药液质量浓度为1.0×10-4g/mL时都具有较好的除草活性,部分化合物在5.0×10-5g/mL时显示出良好的杀菌活性.     

2-氧代-2-[1-（3-吡啶甲基氨基）-1＇-芳基]甲基-4-芳基-5，5-二甲基-1，3，2-二氧磷杂环己烷的合成与生物活性

采用环状亚磷酸酯与亚胺的加成反应, 合成了9个未见文献报道的含吡啶基的α-氨基环状膦酸酯化合物. 其结构经1H NMR, 31P NMR, MS 和元素分析确证, 同时采用X射线单晶衍射对化合物3i的立体构型进行了进一步确证. 测定了该系列化合物的杀虫、杀菌和除草活性, 结果表明, 化合物的杀虫活性虽然较差, 但所有化合物在药液质量浓度为1.0×10-4 g/mL时都具有较好的除草活性, 部分化合物在5.0×10-5 g/mL时显示出良好的杀菌活性.     

Pr3+或La3+与克拉红霉素对大肠杆菌的协同作用

用LKB-2277生物活性检测系统采用停流法于37℃测定了克拉红霉素及克拉红霉素分别与Pr(NO3)3和La(NO3)3混合后,对大肠杆菌生长抑制作用的热效应变化.根据热动力学模型进行了定量解析,得到了各体系的克拉红霉素浓度c与大肠杆菌生长速率常数k之间关系式及其半抑制浓度Ic50.克拉红霉素:k=0.03106-1.273×10-3cIc50=8.81μg·mL-1(0.5～20μg·mL-1)克拉红霉素+Pr3+:k=0.02967-1.332×10-3cIc50=7.38μg·mL-1(1～15μg·mL-1)克拉红霉素+La3+:k=0.02741-1.194×10-3cIc50=6.34μg·mL-1(1～15μg·mL-1)微量热结果不仅表征了克拉红霉素的抗菌活性强于红霉素,Pr3+或La3+与克拉红霉素协同作用也使抗菌活性增强,而且反映了不同药物作用下细菌的生理、生化和代谢过程热动力学特征的变化.     

含噻二唑环苯甲酰脲化合物的合成及杀虫活性

用活性亚结构连接法设计合成了6个新的含1，3，4-噻二唑杂环苯甲酰脲类化合物，其结构经红外光谱、核磁氢谱、元素分析方法确证。同时对其杀虫活性进行了初步研究，发现该类化合物在普筛浓度下对淡色库蚊幼虫具有较好的杀虫活性。化合物Ⅲb(R1=Cl,R2=n-C5H11),Ⅲd(R1=CH3,R2=n-C5H11),Ⅲf(R1=2,6-difluoro,R2=-C5H11)在10mg/L浓度下对淡色库蚊幼虫的杀虫死亡率大于90％。     

Synthesis and Urease Inhibition Studies of Barbituric and Thiobarbituric Acid Derived Sulphonamides

Various novel barbituric and thiobarbituric acid derived sulphonamides were synthesized in excellent yield via three components single pot reaction; and these were screened for in vitro urease inhibition studies against jack bean urease. The compounds 1‐7 were found to exhibit a low to moderate activity whereas compounds 8‐14 showed a significant activity (88.3‐99.9% inhibition determined at 500 μM concentration). Structures of the synthesized compounds were confirmed by ¹H‐NMR, ¹³C‐NMR, mass spectrometry and elemental analysis data.     

Cyanoacetamide Intermediate in Heterocyclic Synthesis: Synthesis and Biological Evaluation of Hitherto New Dioxoisoindoline Heterocyclic Derivatives

Innovative poly‐substituted heterocyclic rings incorporating dioxoisoindoline ( 2 – 25 ) were synthesized through the reaction of dioxoisoindoline derivative 2 as starting compound with various types of reagents. All compounds were characterized by appropriate means of (¹H‐NMR, ¹³C‐NMR, IR, and mass). The prepared compounds were evaluated as antimicrobial agents against Escherichia coli, Staphylococcus aureus, and Candida albicans microorganisms. The tested compounds exhibited low to moderate antibacterial activities and promising results as antifungal agents.     

Design,Synthesis, and Biological Screening of Novel Anthranilic Diamides

Three series of new anthranilic diamide derivatives containing sulfide, N‐cyanomethylsulfilimine, and N‐cyanomethylsulfoximine groups were designed and synthesized by combining the active substructures of anthranilic diamides and sulfoxaflor. The structures of all newly synthesized compounds were confirmed by IR and ¹H/¹³C‐NMR, and some of them were confirmed by elemental analysis or HRMS too. The synthesized compounds were screened for their insecticidal and fungicidal activities. Bioasssay results indicated that some of the synthesized compounds possessed certain degrees of insecticidal activity against Mythimna separata. However, some compounds exhibited good fungicidal activity against Sclerotinia sclerotiorum.     

Pyrido[1,2‐a]pyrimidin‐4‐ones: Ligand‐based Design,Synthesis, and Evaluation as an Anti‐inflammatory Agent

In the present study, a series of novel pyrido[1,2‐a]pyrimidin‐4‐one derivatives ( 1 – 45 ) were synthesized, characterized, and evaluated for their anti‐inflammatory activity. The structures of all newly synthesized compounds were confirmed by ¹H NMR, ¹³C NMR, mass spectroscopy, and C, H, and N analyses. Preliminary these newly synthesized compounds were evaluated for their in vitro cyclooxygenase (COX)‐2/COX‐1 inhibitory activity. The celecoxib, a COX‐2 inhibitor, was used as a reference standard drug. In this inhibitory study, compounds 42 , 43 , 44 , and 45 were found to have significant in vitro inhibitory profile as compared with the reference drug. These compounds were then subjected to their in vivo anti‐inflammatory assay by using carrageenan‐induced rat paw edema method in next level of screening. Later, these same compounds were tested for their ulcerogenic property. Based on these activity data, the compound 43 (in vitro COX‐2 activity—IC₅₀ = 0.4 μM, SI = 400, in vivo anti‐inflammatory activity—72% inhibition after 3 h, and 0.38%—Ulcer index) was emerged as most promising anti‐inflammatory agent with very low ulcerogenic action.     

Facile Synthesis of 3,6‐Disubstituted‐1,2,4‐triazolo‐[3,4‐b]‐1,3,4‐thiadiazoles via Oxidative Cyclization of n‐Heteroaryl‐Substituted Hydrazones and Their Biological Activity

Fused 3,6‐disubstituted triazolothiadiazoles were synthesized in good yield from a rapid and convenient oxidative cyclization of N‐heteroaryl‐substituted hydrazones promoted by chloramine‐T trihydrate at ambient temperature. The structure of the synthesized compounds was confirmed by FTIR, ¹H NMR, ¹³C NMR, and mass spectral data. The synthesized compounds were evaluated for their antioxidant and antitubercular activities. All the compounds 5a‐i and 6a‐i showed good antitubercular activity. However, only compounds 5a‐i showed good antioxidant activity.     

Synthesis,Crystal Structure,and Biological Activity of Novel Anthranilic Diamide Insecticide Containing Propargyl Ether Group

In search of environmentally benign insecticides with high activity, low toxicity, and low residue, a series of novel anthranilic diamide containing propargyl ether were designed and synthesized. All compounds were characterized by ¹H NMR spectroscopy, high‐resolution mass spectrometry, or elemental analysis. The single crystal structure of 18g was determined by X‐ray diffraction. The insecticidal activities against Lepidoptera pests of the new compounds were evaluated. Their insecticidal activities against oriental armyworm (Mythimna separata) and diamondback moth (Plutella xylostella) indicated that most of the compounds showed moderate to high activities at the tested concentration.     

Design,Synthesis, Structure‐Activity Relationship and Insecticidal Activities of Trifluoromethyl‐Containing Sulfiliminyl and Sulfoximinyl Phthalic Acid Diamide Structure

Due to a novel mode action, low toxicity to mammals and low residue characteristics, phthalic acid diamides have aroused considerable interests in agricultural chemistry. With introduction of N‐cyano, N‐trifluoroacetyl, N‐carbamoylsulfiliminyl and sulfoximinyl substituents into phthalamides, 12 novel derivatives containing trifluoromethyl moiety were designed and synthesized. All title compounds were characterized by ¹H NMR and high‐resolution mass spectrometry. The preliminary results of biological activity assessment indicated that some title compounds exhibited moderate to good insecticidal activities against oriental armyworm (Pseudaletia separata Walker). In particular, Va gave higher activity against oriental armyworm and diamondback moth. The present work reported that the new trifluoromethylated diamides incorporating N‐trifluoroacetylsulfoximinyl moieties are potential lead compounds for further structure optimization, providing some insight into the relating structure‐activity relationship.     

Synthesis and Antimicrobial Activity of 2-Methyl-5-nitroaniline Derivatives:A Structure-Activity Relationship Study

A series of 2‐methyl‐5‐nitroaniline derivatives, 5a – 5k and 6a – 6f , were synthesized in order to determine their in vitro antimicrobial activity. The chemical structures of the synthesized compounds were confirmed by elemental analyses, UV‐visible, FT‐IR, ¹H NMR and ¹³C NMR spectral studies. The structure‐activity relationships of the synthesized compounds were also discussed. Among the synthesized compounds, 5f , 5d , 6b and 6e showed good antimicrobial activity compared to standard drugs.     

Synthesis,Dissociation Constants,and Antimicrobial Activity of Novel 2,3‐Disubstituted‐1,3‐thiazolidin‐4‐one Derivatives

In this article, a new series of 2,3‐disubstituted‐1,3‐thiazolidin‐4‐one derivatives have been designed, synthesized, and evaluated as antimicrobial agents. New compounds were prepared by the cyclization reaction of N‐substituted carboxylic acid hydrazide derivatives with mercaptoacetic acid. The structures of the obtained compounds were confirmed by means of IR, ¹H NMR, and ¹³C NMR spectra. The dissociation constants were determined using spectrophotometric method. All synthesized compounds were tested for their in vitro antibacterial and antifungal activities using the broth microdilution method.     

相变温度低且宽的含有胆甾烯基和反式-4-烷基环己基苯氧基的二介晶化合物

Unsymmetrical dimesogenic compounds with cholesteryl and 4-（trans-4-n-alkylcyclohexyl）phenoxy parts were synthesized by condensation of cholester-3-yl 6-bromohexanoate with appropriate 4-（trans-4-n-alkylcyclohexyl）- phenols. Structures and thermal phase behaviour of these dimesogenic compounds have been confirmed by IR, IH NMR, elemental analysis, DSC, polarity microscopy and XRD measurements. Their thermal phase behaviour was significantly different with that of other cholesterol-based dimesogens while they exhibited low and wide phase transition temperature.