Microwave-assisted Synthesis and Crystal Structure of 3-Acetamido-1-phenyl-4-（2,6-dichloro）benzylidene-5-pyrazolone

The title compound,3-acetamido-1-phenyl-4-(2,6-dichloro)benzylidene-5-pyrazolone(C18H13Cl2N3O2,Mr = 374.21),has been synthesized by one-step condensation of 2,6-dichloroben-zaldehyde with acetic anhydride and 3-amino-1-phenyl-5-pyrazolone under microwave irradiation.The compound was characterized by means of IR and 1H NMR.Its crystal and molecular structure were determined by X-ray diffractometry.It belongs to the orthorhombic system,space group Pbca,with a = 12.5312(13),b = 8.5495(9),c = 31.110(3) ,V = 3332.9(6) 3,Z = 8,Dc = 1.492 g/cm3,λ = 0.71073 ,μ(MoKα) = 0.407 mm-1,F(000) = 1536,the final R = 0.0394 and wR = 0.0984.A total of 15894 reflections were collected,of which 3630 were independent(Rint = 0.0362).There exist three planes in the molecular structure.X-ray analysis reveals that the dihedral angles between planes 1 and 2,1 and 3 and 3 and 2 are 80.89,74.29 and 20.57°,respectively.     

A Two-dimensional Metallic Oxide Constructed from Molybdenum Clusters and Ag（Ⅰ）-[3-（2-pyridyl）-pyrazole] Cationic Coordination Components

A new polyoxomolybdate compound [Ag 3 (HL) 4 ](PMo 12 O 40)] 1 (HL=3-(2-pyridyl)pyrazole) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.375(3),b=12.076(3),c=13.196(4),α=84.170(4),β=71.961(3),γ=86.326(4)°,V=1563.1(7)3,C 32 H 28 Ag 3 Mo 12 N 12 O 40 P,M r=2726.52,D c=2.897 g/cm 3,μ(MoKα)=3.366 mm 1,F(000)=1284,Z=1,the final R=0.0587 and wR=0.1312 for 4139 observed reflections (I > 2σ(Ⅰ)).X-ray diffraction analyses reveal that the PMo 12 O 40 3clusters in compound 1 are linked by four Ag 3 (HL) 4 3+ units via the terminal oxygen atoms to form a two-dimensional architecture.The symmetrical unit of Ag 3 (HL) 4 3+ exhibits two distinct Ag(Ⅰ) environments:a two-coordinate {AgN 2 } site and a five-coordinate {AgN 3 O 2 } site which links to two molybdate clusters.     

Synthesis and Crystal Structure of a Dinuclear Complex of Cu（II） with Tetra（3,5-diphenyl pyrazole）

A Cu(II) complex of tetra(3,5-diphenyl pyrazole) [Cu(C15H12N2)2Cl2]2 (1) was synthesized, and its structure was determined by single-crystal X-ray diffraction and further characterized by elemental analysis, NMR and IR. 1 belongs to the monoclinic system, space group P21/c with a = 13.3780(5), b = 15.1392(6), c = 15.5923(6) , β = 124.522(2)°, Z = 2 and V = 2601.86(17) 3. In 1, each Cu2+ ion is coordinated with two N atoms from two tetra(3,5-diphenyl pyrazole) ligands and three Cl- anions to give a distorted square-pyramidal geometry, which is further linked through edge-sharing bridging by Cl- anions to form a centrosymmetric dinuclear structure.     

Structure and Luminescent Properties of the First Cadmium Complex with Isophthalate and Di-pyrazole Ligands

The title complex [Cd(IPA)L(H2O)]n(1,H2IPA = isophthalic acid,L = 1,4-bis(pyra-zole-1-ylmethyl)benzene) has been hydrothermally synthesized,and characterized by elemental analyses,IR spectroscopy,TGA and X-ray single-crystal diffraction.It crystallizes in the triclinic system,space group P1 with a = 9.3060(6),b = 10.2374(7),c = 11.9706(8) ,α = 73.804(6),β = 77.883(5),γ = 85.942(5)°,V = 1070.7(1) 3,Z = 2,C22H20CdN4O5,Mr = 532.82,Dc = 1.653 g/cm3,μ = 1.062 mm-1,λ(MoKα) = 0.71073 ,F(000) = 536,R = 0.0392 and wR = 0.0640 for 3751 observed reflections with I > 2σ(I).Crystal structure analysis showed that complex 1 has a 1D double chain structure,which is assembled together through strong O-H...O hydrogen bonding interactions between coordinated water molecules and carboxylate groups of isophthalate to form a 2D supramolecular network.In addition,the solid-state fluorescent spectrum of 1 exhibits strong emission at 364 nm.     

取代基对3(5)-(9-蒽基)吡唑光学性质的影响

使用密度泛函理论(DFT)B3LYP/6-31G(d)方法优化得到了3(5)-(9-蒽基)吡唑及其衍生物的基态(S₀)分子结构, 使用单激发组态相互作用(CIS)/6-31G(d)方法优化得到这些分子的第一单重激发态(S₁)的几何结构, 并使用含时密度泛函理论(TD-DFT)B3LYP/6-311++G(d,p)方法计算了它们的吸收和发射光谱. 计算结果表明, 与3(5)-(9-蒽基)吡唑相比, 无论取代基是吸电子基团还是供电子基团, 衍生物的吸收和发射峰均发生红移, 并且当取代基―R=―BH₂, ―CCl₃, ―CHO, ―NH₂时衍生物有较长的吸收波长和发射波长.     

"一锅煮"合成新型含吡唑与苯并噻唑环的α-氨基膦酸酯衍生物

在微波辅助、无溶剂、无催化剂条件下,以取代吡唑甲醛,2-氨基苯并噻唑和亚磷酸二乙酯为原料,"一锅煮"合成了6个新型含吡唑与苯并噻唑环的α-氨基膦酸酯衍生物,其结构经1H NMR,13C NMR和MS表征.     

茂铁基二氢吡唑类衍生物的液相色谱分离研究

本文利用梯度洗脱进行溶剂强度的优化,确定分离一组化合物的最佳二元流动相体系,即甲醇-水、四氢呋喃-水和乙腈-水,将这三种二元流动相的最佳组成作为溶剂选择性三角形的三个顶点,利用ORM法对流动相进行优化选择,得到流动相的最佳组成和配比为V乙腈:V四氢呋喃:V水=33.75:33:33.25,有效地分离了六种二茂铁取代二氢...     

多壁碳纳米管-酰基吡唑啉酮复合膜修饰电极测定异烟肼

报道了一种修饰电极--多壁碳纳米管-酰基吡唑啉酮复合膜修饰玻碳电极(MWNTs/HPMαFP/GCE ),研究了异烟肼在此修饰电极上的电化学行为及反应机理.与裸GCE和MWNTs/GCE相比,异烟肼在MWNTs/HPMαFP/GCE上的氧化峰电流和检测灵敏度大大提高,表明多壁碳纳米管和酰基吡唑啉酮产生了协同增效作用.在...     

1-[6-(3,5-二甲基-1H-吡唑-1-基)-1,2,4,5-四嗪-3-基]酰肼及其衍生物的合成与表征

以水合肼和硝酸胍为原料,经肼化、环化、氧化和肼化四步反应合成了1-[6-(3,5-二甲基-1H吡唑-1-基)-1,2,4,5-四嗪-3-基]酰肼(4);4与酰氯或磺酰氯反应合成了一系列新型的1-[6-(3,5-二甲基-1H-吡唑-1-基)-1,2,4,5-四嗪-3基]酰肼衍生物(6a～6j),其结构经1H NMR,IR...     

1，3—Diphenyl—5—（9—phenanthry1）—2—pyrazoline（DPPhP）：An Excellent Ho1e—Transport Material for Use in Organic Light—Emitting Diodes

An excellent hole-transport material,1,3-diphenyl-5-(9-phenanthryl)-2-pyrazoline(DPPhP)for OLEDs was studied.This compound not only offers hlgh glass transition temperature(Tg=96℃）,good film forming ability,and high HOMO energy level,but also displays excellent hole-transport property.The electrlumlnescent device with a simple structure of ITO/DPPhP(60nm)/AIQ(60mm)/LiF(0.8nm)/Al shows an external quantom efficiency as high as 1.6?