邻-吡啶苯并噻二唑衍生物的合成与双光子荧光传感性能

以吡啶苯并噻二唑基元为荧光传感"接受体(齿)",将其与咔唑"核"键合获得单齿和双齿两个化合物:2,8-(2-吡啶苯并噻二唑)-N-乙基氮杂笏(CPTZ1)和2,8-双(2-吡啶苯并噻二唑)-N-乙基氮杂芴(CPTZ2),并通过红外光谱、核磁共振谱、质谱表征.通过稳态/瞬态单光子荧光测试和飞秒钛宝石激光器泵浦探测,探讨了CPTZ1和CPTZ2化合物对质子[H+]的敏感性.Stern-Volmer方程给出CPTZ1的单、双光子荧光的猝灭常数分别为:k1PSV=0.04 L·mol-1,k2PSV=0.20 L·moL-1;而CPTZ2的猝灭常数则分别为k1PSV=0.10 L·moL-1,k2PSV(CPTZ2)=0.22 L·moL-1.研究结果表明,双光子荧光(TPF)检测表现出对质子更高的敏感性,其灵敏度是相应的单光子荧光(OPF)的2～5倍.     

Synthesis and biological evaluation of novel 1,2,4-triazole containing 1,2,3-thiadiazole derivatives

A series of novel 1,2,4-triazoles containing 1,2,3-thiadiazole derivatives were designed and synthesized. Their structures were confirmed by melting points, IR, 1H NMR, and elemental analysis and ESI-MS or HRMS. Preliminary bioassays indicated that these compounds exhibited very good insecticidal activity against Aphis laburni at 100 μg/mL, with mortality no less than 95%. Compounds 6a, 6c, 6f, 61 showed higher curative activity against TMV and compound 6h showed a higher induction effects against TMV in vivo at 100 μg/mL. Collectively, our data demonstrate a new strategy for control of insects and viruses.     

Synthesis,Crystal Structure,and Biological Activity of Naphthalen-2-yl4-methyl-1,2,3-thiadiazole-5-carboxylate

The title compound naphthalen-2-yl-4-methyl-1,2,3-thiadiazole-5-carboxylate (C 14 H 10 N 2 O 2 S,M r=270.31) was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1 H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a=23.475(5),b=9.6640(19),c=10.814(2),β=90.00°,Z=8,V=2453.2(9) 3,M r=270.30,D c=1.464 g/cm 3,μ=0.262 mm-1,F(000)=1120,R=0.0444 and wR=0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6) H(6)···O(1) and C(14) H(14)···O(1) were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.     

Synthesis,Crystal Structure and Biological Activity of N-（2,6-Difluorobenzoyl）-N＇-[5-（4-trifluoromethyl-phenyl）-1,3,4-thiadiazol-2-yl]ure

The title compound N-(2,6-difluorobenzoyl)-N'-[5-(4-trifluoromethylphenyl)-1,3,4-thiadiazol-2-yl]urea(C17H9F5N4O2S,Mr = 428.34) has been synthesized by the reaction of 2-amino-5-(4-trifluoromethylphenyl)-1,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate,and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n with a = 10.7316(13),b = 10.5617(13),c = 16.037(2) ,β = 106.408(2)°,V = 1743.6(4) 3,Z = 4,Dc = 1.632 g/cm3,μ = 0.260 mm-1,F(000) = 864,the final R = 0.0599 and wR = 0.1420 for 3467 observed reflections with I > 2σ(I).The urea group,which adopts a planar configuration mediated by the intramolecular N-H...O hydrogen bond,is nearly coplanar with the thiadiazole and 4-trifluoromethylbenzene rings.The title compound was found to exhibit good fungicidal activity against Rhizoctonia solani and Botrytis cinerea.     

球状壳聚糖负载噻二唑树脂的合成及其吸附性能

用苯甲醛保护胺基后,将2-氨基-5-巯基-1,3,4-噻二唑引入到大孔壳聚糖微球上,合成了亲水性的多孔球状吸附树脂(CTS-AMT)。 对比研究了CTS-AMT和母体微球(CTS)对Zn2+、Cu2+、Cd2+、Pb2+、Ag+和Hg2+的吸附性能。 结果表明,pH=5.0,T=298.15 K时,CTS-AMT树脂对上述金属离子的吸附在1.5 h内基本达到平衡,对金属离子Hg2+、Ag+和Pb2+的静态饱和吸附量分别为2.54、2.31和1.71 mmol/g。 在实验浓度范围内该树脂对Hg2+的吸附过程符合 Langmuir等温吸附模型。     

微波法合成1,ω-二(2,2-二氨基-1,3,4-噻二唑-5-)烷烃类化合物

以浓硫酸为催化剂,氨基硫脲(1)与二元羧酸(2a～2d)在微波辐射下经环合反应合成了四种新型的1,ω-二(2,2-二氨基-1,3,4-噻二唑-5-)烷烃类化合物,其结构经1H NMR和IR表征.最佳反应条件为:1 20mmol,n(1):n(2)=2.0:1.8,浓硫酸2.6 mL,中低火微波辐射6 min,产率77....     

含1,2,3-噻二唑的邻甲酰胺基苯甲酰胺类化合物的合成、晶体结构与生物活性

以取代邻氨基苯甲酸为起始原料, 设计并合成了一系列未见文献报道的含1,2,3-噻二唑的邻甲酰胺基苯甲酰胺类化合物. 所有化合物的结构均经元素分析和1H NMR确证, 并且采用X射线单晶衍射分析方法测定了化合物7g的结构. 初步的生物活性试验结果表明, 部分化合物具有一定的杀菌活性.     

2,5-二(邻羟苯基)-1,3,4-噻二唑与镍的显色反应及应用

由于光度法具有操作简便、仪器价廉等优点,近年来,利用合成新显色剂显色测定镍的报道也有不少[1-4],但噻二唑类试剂用于光度分析的报道却很少。2,5-二(邻羟苯基)-1,3,4-噻二唑是自合成的试剂,该试剂性质稳定,其溶液近似无色,具有较好的光度分析选择性,只与常见离子Cu2 ,Co2 ,Ni2 ,VO2 ,Ag 显色。该试剂与镍显色灵敏度较高,线性范围宽,结合合适掩蔽剂的使用,用于环境水样和茶叶中镍的测定,获得了满意的结果。1试验部分1.1主要仪器与试剂721分光光度计;Cintra 10型紫外可见光谱仪;pHS-3C精密酸度计。镍标准储备溶液:1.0 g·L-1,使用时稀…     

含1,3,4-噻二唑结构的酰胺类衍生物的合成及生物活性研究

随着养殖技术不断提高，水产养殖向高密度、集约化发展的同时，养殖水产品弧菌所引起的疾病也日趋严重，这类疾病不仅给水产养殖业带来了巨大的损失，也引起了人们的饮食健康问题，因此，水产养殖业对于新型安全高效抗菌药的需求迫在眉睫。以醛类化合物为原料，与硫代氨基脲形成希夫碱类化合物，成环后生成1,3,4-噻二唑类衍生物，并与不同链长的酰氯反应，合成6个含1,3,4-噻二唑结构的酰胺类衍生物，所有化合物的结构经IR、¹H NMR以及HR-MS(ESI)确证。采用牛津杯法测试目标化合物对霍乱弧菌和副溶血弧菌的抑菌圈直径及最小抑菌浓度(MIC)。生物活性测试结果表明：化合物4b对霍乱弧菌的抑菌圈直径为11.79±0.15 mm,化合物4a和4c哈维氏弧菌的抑菌圈直径分别为17.53±0.08 mm、 19.37±0.56 mm, MIC均为0.25 mg·mL^-1。化合物4a、4b和4c对海洋弧菌具有较好抑制活性，可为后续水产抗菌药物的研发提供理论基础。