Synthesis of novel pyrazole‐based triazolidin‐3‐one derivatives by using ZnO/ZrO2 as a reusable catalyst under green conditions

An efficient approach for the synthesis of 10 novel pyrazole‐based 1,2,4‐triazolidin‐3‐one derivatives catalyzed by ZnO‐loaded ZrO₂ as heterogeneous catalyst with ethanol as solvent is described. The structure of the mixed metal oxide catalyst was characterized by various instrumental techniques (scanning electron microscopy, transmission electron microscopy, X‐ray diffraction and Brunauer–Emmett–Teller). In smooth reactions, products were accomplished in excellent yields (90–94%) with short reaction times (≈ 45 min). ZnO/ZrO₂ catalyst exhibited good recyclability. The catalyst is reused six times without any noticeable loss of activity. The major advantages of this method are operational simplicity, mild conditions, simple work‐up procedure and broad functional group tolerance.     

Synthesis,Crystal Structure and Antifungal Activities of 3-Methyl-l-（4-methylphenyl）-4- （N-4-trifluoromethylphenyl）-aminomethyl- 5-（4-methoxyphenylthio）-lH-pyrazole

The title compound 3-methyl-l-（4-methylphenyl）-4-（N-4-trifluoromethylphenyl） aminomethyl-5-（4-methoxyphenylthio）-lH-pyrazole has been synthesized via a four-step reaction and characterized by IR, 1H NMR, elemental analysis and X-ray crystallography. The compound crystallizes in monoclinic, space group P21/c with a = 8.7170（15）, b = 18.355（3）, c = 15.292（3） A, fl = 103.445（3）°, V= 2379.7（7） A3, Dc = 1.350 g/cm3, Z = 4, p = 0.184, F（000） = 1008, and the final R = 0.0491 and wR = 0.1339 for 4160 observed reflections （I 〉 2a（/））. The results demonstrate that there is a face-to-face π-π stacking interaction between one benzene ring （C（19）-C（24）） and another （C（I 3）-C（! 8）） at a plane-plane distance of 3.3539 A. The ring normal and vector between the ring centroids form an angle of 18.2° up to the centroid-to-centroid distance of 3.5273 A. The crystal structure is stabilized by the intermolecular hydrogen bond of N（3）-H（3A）...N（2） （symmetry code： A -x＋l, -y＋l, -z）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

新型含吡唑基双噁二唑啉衍生物的合成与表征

基于药物设计中的活性叠加原理,以α-氯代-4-取代苯甲醛肟和对苯二酚为起始原料,经过一系列的反应,将1,2,4-噁二唑环引入到吡唑环中,合成了16种新型含吡唑基双噁二唑啉衍生物,并通过IR,MS,1 H-NMR对这些化合物进行了表征.     

含吡唑基的苯骈咪唑的合成与光谱性能(英文)

在乙醇溶剂中,于温和条件下以邻苯二胺和1-苯基吡唑-4-醛为原料合成了一种结构新颖的含吡唑取代基的苯骈咪唑杂环化合物,通过元素分析,MS,1H NMR对所合成的苯骈咪唑化合物的组成与结构进行了表征,同时对该化合物的紫外-可见光谱和荧光光谱进行了研究.     

Oximes of five-membered heterocyclic compounds with two heteroatoms 2. Reactions and biological activity (Review)

Data on the reactions of oxazole, thiazole, pyrazole, and imidazole aldoximes, ketoximes, amidoximes, and their derivatives are reviewed. The synthesis of new heterocycles based on the oximes of five-membered heterocyclic compounds with two heteroatoms are considered separately. The principal results from investigation of the biological activity of the ethers of these oximes are also presented. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1123–1155, August, 2007.     

单晶Ni(Pyrazole)_4X_2(X=C1,Br)的光谱研究

本文利用d8（D2h*）全组态强场近似理论，对单晶Ni（pyrazole）4X2（X=C1，Br）型化合物的光谱进行了理论计算，计算结果与实验符合较好。     

超声法合成新型3-(5-氯/苯氧基-3-甲基-1-苯基-4-吡唑基)异噁唑N-取代苯基去甲去氢斑蝥酰亚胺衍生物

去甲去氢斑蝥素与取代芳胺反应得到了一系列N-取代苯基去甲去氢斑蝥酰亚胺, 再与5-氯/苯氧基-4-(α-氯-α-肟基甲基)-3-甲基-1-苯基吡唑甲酰基氯代肟发生1,3-偶极环加成反应生成一系列未见报道的3-(5-氯/苯氧基-3-甲基-1-苯基-4-吡唑基)异噁唑N-取代苯基去甲去氢斑蝥酰亚胺衍生物. 所合成化合物经元素分析, IR, ¹H NMR, ¹H-¹HCOSY, NOESY确证结构.     

1-吡唑酰基-4-芳基氨基脲类化合物的合成及除草活性

为了寻求新的含吡唑氨基脲先导化合物, 用4-溴-1-甲基-3-乙基-5-吡唑甲酰肼与取代苯基异氰酸酯反应得到了14个新的含吡唑氨基脲类化合物. 经IR, ¹H NMR, MS和元素分析对化合物的结构进行了表征. 初步生物活性实验结果表明, 在225 mg/m²浓度下, 1-(1-甲基-3-乙基-4-溴-5-吡唑甲酰基)-4-(2,4-二甲基苯基)氨基脲(4k)对苘麻(Abutilon theophrasti)、藜(Chenopodium album)及刺苋(Amaranthus spinosus)抑制活性达到100%.     

3-芳氧基-6-(3,5-二甲基-1H-吡唑-1-基)哒嗪的合成及生物活性

为了寻找高活性的先导化合物, 以3,6-二氯哒嗪为原料, 经过三步反应, 合成了一系列未经文献报道的3-芳氧 基-6-(3,5-二甲基-1H-吡唑-1-基)哒嗪. 所有新化合物的结构均经过¹H NMR, IR, LC-MS和元素分析确认. 初步的生物活性测试表明, 所合成的化合物都有一定的除草活性.     

取代吡唑-5-酰基杂环衍生物的合成、结构与生物活性

为了寻求新的含吡唑双杂环先导化合物. 用4-取代-1-甲基-3-乙基-5-吡唑甲酰氯与2-噻唑烷酮、2-噻唑硫酮、2-噁唑烷酮等含氮杂环反应得到了12个含吡唑环的双杂环化合物. 化合物结构用IR, ¹H NMR, MS和元素分析进行了表征. 并用X射线单晶衍射法测定了化合物3-(1-甲基-3-乙基-4-硝基-5-吡唑甲酰基)-噁唑烷-2-酮(3k)的晶体结构. 晶体为单斜晶系, P2₁/n (#14)空间群, a＝1.52175(3) nm, b＝0.52970(1) nm, c＝1.58185(3) nm, β＝104.893(4), V＝1.2323(4) nm³, Z＝4, D_c＝1.45 g/cm³, F(000)＝560.00, R₁＝0.064, wR₂＝0.193. 初步生物活性实验结果表明, 在25 mg/L浓度下, 3-(1-甲基-3-乙基-4-硝基-5-吡唑甲酰基)-噻唑烷-2-酮(3c), 3-(1-甲基-3-乙基-4-硝基-5-吡唑甲酰基)-噻唑烷-2-硫酮(3g)对水稻稻瘟病菌(Pyricularia oryzae)的抑制活性达到40%. 在500 mg/L浓度下, 3-(1-甲基-3-乙基-4-溴-5-吡唑甲酰基)-噻唑烷-2-酮(3d), 3-(1-甲基-3-乙基-4-溴-5-吡唑甲酰基)-噁唑烷-2-酮(3l)对稻黑尾叶蝉(Nephotettix cinc-ticeps)的抑制活性达到53.37%.