2—氯／2—甲磺酰基—5—（2—苯基—4—喹啉基）—1,3,4—恶二唑…

借处理２－羟基－５－（２－苯基－４－喹啉基）－１，３，４－恶二唑同ＰＣｌ５／ＰＯＣｌ３之间的反应合成了２－氯－５－（２－苯基－４－喹啉基）－１，３，４－恶二唑（３）和通过２－Ｙｕ基－５－（２－苯基－４－喹啉基）－１，３，４－恶二唑的甲基化，然后氧化制得２－甲磺酰基－５－（２－苯基－４－喹啉基）－１，３，４－恶二唑（６）。并分别研究了３和６同胺、叠氮及肼的反应，得到２，５－二取代的恶二唑新衍生物。初     

2，5－二取代－1，3，4－噁二唑类化合物的合成

扼要综述了近年来关于１，３，４－噁二唑类化合物的新的合成方法，讨论了相应合成反应的机制。     

1－（取代异噁唑基）－1，2，4．三唑和1－（取代嘧啶基）－1，2，4－三唑的合成及生物活性

合成了１５个新的１－（取代异噁唑基）－１，２，４－三唑和１－（取代嘧啶基）－１，２，４－三唑化合物，经元素分析、ＩＲ、１ＨＮＭＲ和ＭＳ证实其结构，并对其代表化合物进行了抑菌及植物生长调节活性的初步观察     

含氮亲核试剂在2-甲磺酰基-5-(3,4,5-三甲氧基苯基)-1,3,4-噁二唑环上取代反应的研究

2,5—二取代—l,3,4—噁二唑化合物具有消炎,抗菌,调节植物生长,杀虫门等广泛的生物活性。作者曾研究了取代胺在2—甲磺酰基—5—(2—苯基—4—喹啉基)—1,3,4—噁二唑化合物环2—位上的亲核加成消去反应,制得了一系列新的2—取代基—5—(2—苯基—4—喹啉基)—1,3,4—噁二唑衍生物,并发现它们具有一定的抗菌活性。在此基础上,我们又研究了含氮亲核试剂在 2—甲磺酰基—5—(3,4,5—三甲氧基苯基)—1,3,4,—噁二唑环2—位上的亲核加成消去反应,制得一系列新的2—取代基—5—(3,4,5—三甲氧基苯基)—1,3,4—噁二唑衍生物。作者用3,4,5—三甲氧基苯甲酰肼在KOH催化下与CS_2反应得到2—巯基—5—(3,4,5—三甲氧基苯基)—l,3,4—噁二唑1,1在NaOH溶液中与Me_2S0_4作用得到2—甲硫醚—5—(3,4,5—三甲氧基苯基)—1,3,4—噁二唑2,2在冰醋酸水溶     

2-芳氧基-5-苯基-1,3,4-噁二唑类化合物的合成

本文通过芳氧基负离子在2—甲磺酰基—苯基—1,3,4—噁二唑环2—位上的亲核取代反应制得9个新的2—芳氧基—5—苯基—l,3,4—噁二唑衍生物。所有化合物的结构经元素分析,IR,~1H NMR和MS确认。初步抗菌实验表明这些化合物具有一定的抑制枯草芽孢杆菌繁殖的活性。 2,5—二取代l,3,4—噁二唑衍生物具有广泛的生物活性,如抗菌,抗黄球菌,除草杀棉花牙虫等。Madhavan等曾通过芳胺在2— 甲磺酰基—5—芳基1,3,4—噁二唑环上的亲核取代反应,制得了2—芳氨基—5—芳基—l,3,4—噁二唑衍生物,我们也曾通过酰肼等亲核试剂在2—甲磺酰基—5—(3,4,5—三甲氧基苯基)—1,3,4—噁二唑环上的亲核取代反应,得到了2—取代酰肼基—5—(3,4,5—三甲氧基苯基)—l,3,4—噁二唑衍生物。在此基础上,我们拟通过Aro在2—甲磺酰基     

含1，3，4-噁二唑取代的酰基硫脲的合成及杀菌活性

大量文献报道了1，3，4-噁二唑的合成及广泛的生物活性，酰基硫脲类化合物也因其广谱的生物活性引起了人们浓厚的研究兴趣。根据活性因子叠加的原理，本文将一系列1，3，4-噁二唑引入到酰基硫脲中，从对氯苯氧乙酸出发，得到的酰基异硫氰酸酯再与一系列2-氨基-5-芳基-1，3，4-噁二唑反应，合成了10个酰基硫脲类化合物。所有化合物均经元素分析、红外光谱、核磁共振谱和质谱确认。同时对所有化合物进行了生物活性测试。合成路线如下。     

1－（取代吡唑－4－基）－1，2，4－三唑的合成及生物活性研究

合成了２３个新的１－（取代吡唑－４－基）１，２，４－三唑化合物，经ＥＡ、ＩＲ、~１ＨＮＭＲ和ＭＳ确定其组成和结构，并对其进行了抑菌及生长调节活性的初步观察。     

(3-苄基-4-芳酰基-1,2,4-三唑-5-基)(5-本基-1,3,4-噁二唑-2-基)硫醚的合成

通过3-苄基-4-芳酰基-1,2,4-三唑-5-巯基负离子在2-甲磺酰基-5-苯基-1,3,4-噁二唑环2-位上的亲核取代反应,制得13个新的(3-苄基-4-芳酰基-1,2,4-三唑-5-基)(5-苯基-1,3,4-噁二唑-2-基)硫醚衍生物.经元素分析、IR、~1H NMR和MS裂解碎片分析确认结构.初步观察了它们在0.01％浓度时对大肠杆菌繁殖的抑制作用.     

均三嗪基修饰的1，3，4-噁二唑类化合物的合成

1，3，4-噁二唑类材料具有优良的电子传输性及很好的耐热性和抗氧化性，是目前应用最广泛的电子传输材料。然而由于小分子化合物性质不稳定，尤其是其热稳定性差以及易重结晶，从而影响电致发光器件的使用寿命。本文引入均三嗪基团对其进行化学修饰以改善其电子传输性能和稳定性，合成了几种2-苯基-5-(对氨基苯基)-1，3，4-噁二唑取代的二氯均三嗪及其衍生物。合成路线如下。     

含氮亲核试剂在2-甲磺酰基-5-(3,4,5-三甲氧基苯基)-1,3,4-恶二唑环上取代反应的研究

本文报道了制备2-甲磺酰基-5-(3,4,5-三甲氧基苯基)-1,3,4-恶二唑和其进一步与多种亲核试剂反应. 2-巯基-5-(3,4,5-三甲氧基苯基)-1,3,4-恶二唑经过甲基化, 而后用KMnO~4氧化得到2-甲磺酰基-5-(3,4,5-三甲氧基苯基)-1,3,4-恶二唑衍生物. 其结构由元素分析,IR, ^1H NMR 和MS确定.化合物4对大肠杆菌和枯草芽孢杆菌有较强的抑制性能.     

Synthesis of 3-cyano-2-fluoropyridines

The synthesis of 3-cyano-2-fluoropyridines from readily available precursors was achieved via nucleophilic substitution of a leaving group in the 2-postion with KF or Bu₄NF in polar aprotic solvents such as DMF and DMSO. Ionic tetrahydrothiophenium fragment is the most effective leaving group, the methanesulfonyl moiety is a somewhat less effective, and Br- and Cl- are the least effective. Relatively mild conditions of the reaction between (2-pyridyl)-tetrahydrothiophenium salts and KF, as well as the convenience of one-step synthesis of these salts from 2(1H)-pyridinethiones, make these salts the compounds of choice for the preparation of ring-fluorinated pyridines.     

Synthesis of Novel Chiral C2-Symmetric Bisoxazoline Ligands Containing 2,5-Di( m -substituted)phenyl-1,3,4-oxadiazole

Abstract

Seven novel chiral C₂-symmetric substituted bisoxazoline ligands containing 2,5-di(m-substituted)phenyl-1,3,4-oxadiazole have been synthesized from 2,5-di-(m-carboxylphenyl)-1,3,4-oxadiazole and aminoalcohol by NaOH or Et₃N cyclization method via halogenated amide intermediate.     

2-芳基-5-(2-苯基-4-喹啉基)-1,3,4-恶二唑衍生物的合成及其相关性质的研究

1,3,4-恶二唑衍生物在医药,农药、染料、涂料、高分子合成材料以及有机闪烁体材料等方面有广泛用途。近年来有关合成和生理活性的研究报道甚多。本文选择被淘汰的解热镇痛、去风湿药物     

Synthesis and Spectrophotometric Studies of 2-(1, 3, 4 -Triazolylazo) -5-Diethylamino Phenol and 2-(5-Carboxy-1, 3, 4-Triazolylazo) -5- Diethylamino Phenol

Inasearchfornewsensitiveandselectiveorganicreagents,athoroughstudyofsomeofthequinolylazo,pyridylazocompoundshasbeenreported'-'.Buttriazolylazocompoundshavenotbeenstudied.Inthispapef,2-(l,3,4-triazolylazo)-5-diethyIaminophenol(TZAPN)and2-(5-carboxy-l,3,4-triazoiylazo)-diethyIaminophenoI(CTZAPN)wereprepared,theconditionsofthisreactionwithcobaltwerestudied.Itwasfoundthatthereagentshadhighsensitivityandselectivityinthedeterminationofmicrogramamountsofcobaltundertheconditionsestablished.Thest…     

Preparation and characterization of symmetrical bis[4-chloro-2-pyrimidyl] dichalcogenide (S, Se, Te) and unsymmetrical 4-chloro-2-(arylchalcogenyl) pyrimidine: X-ray crystal structure of 4-chloro-2-(phenylselanyl) pyrimidine and 2-(p-tolylselanyl)-4-chloropyrimidine

Synthesis of a novel class of multinucleate pyrimidine chalcogen (S/Se/Te) derivatives has been successfully attempted for the first time by the selective substitution of chlorine at the C-2 position of 2,4-dichloropyrimidine with nucleophilic dichalcogenide anion E₂²⁻ (E = S, Se, Te) to afford bis[4-chloro-2-pyrimidyl] dichalcogenide. The highly electrophilic nature of 2,4-dichloropyrimidine compared to aryl chlorides has been further exploited to prepare a variety of 4-chloro-2-(arylchalcogenyl) pyrimidine compounds by substituting the chlorine exclusively at the C-2 position of 2,4-dichloropyrimidine with a variety of chalcogen bearing aryl anions ArE⁻ (Ar = phenyl, 1-naphthyl, p-tolyl, 4,6-dimethyl-2-pyrimidyl, 2-pyridyl, 4-methyl-2-pyridyl). All the newly prepared symmetrical and unsymmetrical pyrimidyl chalcogen compounds have been thoroughly characterized with the help of various spectroscopic techniques viz., NMR (¹H, ¹³C, ⁷⁷Se), FT-IR and mass spectrometry (in representative cases). The crystal structures of 4-chloro-2-(phenylselanyl) pyrimidine and 2-(p-tolylselanyl)-4-chloropyrimidine have been determined by X-ray crystallography.     

Synthesis,crystal structure and fungicidal activity of 1-(4-chlorophenyl)-2-(5-((3,5-dimethyl-1H-pyrazol-1-yl)methyl)-4-phenyl-4H-1,2,4-triazol-3-ylthio)ethanone

A novel bis-heterocyclic compound was synthesized and characterized. The crystal structure of the title compound (C₂₂H₂₀ClN₅OS, Mr = 437.94) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P-1 with a = 8.646 (2), b = 9.148 (3), c = 14.540 (4) Å, α = 94.422 (4), β = 98.500 (4), γ = 102.823 (4)°, V = 1101.8 (5) Å³, Z = 2, F(000) = 312, Dc = 1.320 g/cm³, μ = 0.2900 mm^?1, the final R ₁ = 0.041000 and wR ₂ = 0.1160 for 2675 observed reflections with I > 2σ(I). A total of 5623 reflections were collected, of which 3866 were independent (R _int = 0.019000). The fungicidal activity of title compound was determined, the results showed the title compound displayed moderate fungicidal activity against G. zeae Petch, Phytophthora infestans (Mont.) de Bary, Botryosphaeria berengeriana f. sp. piricola (Nose) koganezawa et Sakuma, Fusarium oxysporum f.sp. cucumerinum, and Cercospora arachidicola.     

Synthesis of Novel N-carbohydrate-derived Heterocyclic Compounds by Nucleophilic Substitution Reaction of Carbohydrate Imidazole-1-sulfonates

The nucleophilic substitution reaction of carbohydrate imidazole-1-sulfonates with pyrrole and other nitrogen heterocyclic compounds is reported for the first time. Several novel N-carbohydrate-derived heterocyclic compounds have been prepared by this displacement reaction. The desired carbon-nitrogen bond formation proceeds under mild conditions to generate the coupling products in good yields with readily available and inexpensive reagents. This method is particularly suitable for carbohydrate imidazole-1-sulfonates of primary alcohols. Supplemental materials are available for this article. Go to the publisher's online edition of Journal of Carbohydrate Chemistry to view the free supplemental file.     

3-甲基-1-苯基-4-{4-([5-甲基-2-(4-取代芳基)-噁唑-4-基]甲氧基)-芳亚甲(苄)基}-2-吡唑啉-5-酮的设计、合成与降血糖活性

设计合成了具有降血糖活性的3-甲基-1-苯基-4-[4-[[5-甲基-2-(4-取代芳基)-噁唑-4-基]甲氧基]-芳亚甲(苄)基]}-2-吡唑啉-5-酮类化合物.用丁二酮单肟和(取代的)苯甲醛环合、氯化得到氯甲基噁唑衍生物,与对羟基苯甲醛或香兰醛缩合,再与3-甲基-1-苯基-2-吡唑啉-5-酮进行Knoevenagel反应及催化氢化得到目标化合物(Ⅰ和Ⅱ),共合成了16个未见文献报道的新化合物,并利用元素分析、IR、MS和1HNMR确证了化合物的结构.初步药理试验结果表明,所合成的化合物有抑制血糖升高的倾向以及能明显加强和延长外源性胰岛素的降血糖作用,其中化合物Ⅰb,Ⅰd和Ⅰf尤为突出,说明这类化合物可能有增强胰岛素敏感性的作用.     

合成2—芳氧基—5—氟—3H—4—嘧啶酮的新方法

由２－氰－５－氟－３Ｈ－４－嘧啶酮和取代苯酚钠在常压下反应，合成了７个未见文献报道的２－芳氧基－５－氟－３Ｈ－４－嘧啶酮化合物，产率７０￣８７％，结构经ＩＲ、＾１Ｈ ＮＭＲ和ＭＳ证实。