含吡唑啉酮氨基脲类化合物的合成及结构

以1-苯基-3-甲基-吡唑啉酮-5 (PMP)和1,3-二苯基-吡唑啉酮-5 (DPP)为原料合成了六种4-酰基吡唑啉酮,并分别与氨基脲缩合,得到六个新的含吡唑啉酮环的缩氨基脲类化合物.用IR, ¹H NMR和¹³C NMR对各化合物进行了表征及结构确证,并用X射线单晶衍射法测定了化合物1c [1-苯基-3-甲基-4-丙酰基-吡唑啉酮-5缩氨基脲(PMPP-SC)]的晶体结构.     

含吡唑啉酮酰肼类衍生物的合成与结构

报道了PMBP-NTH(NTH为烟酰肼)与PMBP-PAH(PAH为对甲氧基苯甲酰肼)的合成、表征和晶体结构分析,PMBP-NTH晶体属三斜晶系,具有P1空间群,a=0.9024(2)nm,b=1.0953(2)nm,c=1.1635(2)nm,α67.070(10)°,β=68.220(10)°,γ=84.770(10)°,V=0.9816(3)nm^3,Z=2,Dc=1.345g/cm^3,μ=0.090mm^-1,F(000)=416,R=0.0363,ωR=0.0870.PMBP-PAH属单斜晶系,具有P21/c空间群,a=1.2715(4)nm,b=0.91710(10)nm,c=1.8979(3)nm,β=106.890(10)°,V=2.1177(8)nm^3,Z=4,Dc=1.338g/cm^3,μ=0.090mm^-1,F(000)=896,R=0.0414,ωR=0.0972.这两个化合物在分子内都形成了大的共轭体系,由于分子间氢键力的作用,又使它们在晶体中以二聚体形式存在.     

呋喃甲酰基吡唑啉酮缩氨基硫脲稀土配合物的合成、表征及生物活性

合成了含硫席夫碱试剂 1-苯基-3-甲基-4-((-呋喃甲酰基)吡唑啉酮-5缩氨基硫脲(L)及其10种稀土配合物. 元素分析及摩尔电导值表明新配合物的组成为[REL2(NO3)2]NO3(RE= La,Pr,Nd,Sm,Eu,Tb,Dy,Er,Yb,Y. 运用红外光谱、紫外光谱、核磁共振谱和荧光光谱对配合物进行了表征. 抗菌实验表明配合物具有较强的抗菌生物活性.     

几种新的4-酰代吡唑啉酮衍生物的合成与结构

利用4-酰代吡唑啉酮与氨基硫脲类化合物反应制备了新的吡唑啉酮类衍生物,并用IR,NMR,MS和元素分析进行表征,最后用X射线四圆衍射对其中的2个化合物进行了晶体结构测定。     

1-苯基-3-甲基-4-(6-氢-4-甲基氨基-5-硫杂-2,3-吡嗪)-吡唑啉酮的合成与晶体结构

通过1-苯基-3-甲基-4-氯乙酰基-吡唑啉酮-5 (PMCP) 和4-甲基氨基硫脲 (MTSC) 缩合, 形成了一种新的双杂环化合物 (PMCP-MTSC)。利用元素分析与单晶X-射线衍射进行了表征。 该化合物(C14H15N5OS)属单斜晶系, P21 空间群, 晶体学参数为 a = 7.634(1), b = 11.639(2), c = 8.150(2) ? ?= 98.13(1), V = 716.9(2) ?, Z = 2, Dc = 1.396 g/cm3, (MoKa) = 0.232 mm-1, F(000) = 316, Mr = 301.37。结构由直接法解出,共收集3114个衍射点,其中I > 2(I)的独立衍射点有2453个,用全矩阵最小二乘法修正,最终偏离因子:R = 0.0294, wR = 0.0738。结构分析表明: 该化合物以酮式存在,分子间通过氢键作用(N(5)H…O)连接起来并形成一维链状结构。     

苯并噻唑基酰基吡唑啉酮的合成

在非水溶剂中合成了4种新型苯并噻唑基酰基吡唑啉酮试剂。用元素分析、IR、1H NMR和LC-MS对其结构进行了表征。结果显示:不同测试条件下,4个化合物存在方式不尽相同,可主要以酮式或酮式和烯醇式异构体共存方式存在。     

含萘酰亚胺光功能基元的吡唑啉酮席夫碱的合成及其光谱性质

以4-溴-1,8-萘酐为原料,经亚胺化、取代和还原反应合成了中间体N-对氨基苯基-4-哌啶-1,8-萘酰亚胺(4),4与1-苯基-3-甲基-4-苯甲酰基-吡唑啉酮-5缩合得到一种含萘酰亚胺光功能基元的的新型吡唑啉酮席夫碱——1-苯基-3-甲基-4-苯甲酰基-吡唑啉酮-5缩N-对氨基苯基-4-哌啶-1,8-萘酰亚胺(6)。4和6的结构经1H NMR和IR确证。研究了6在不同溶剂中的光谱性质,发现其吸收光谱和荧光光谱随溶剂的极性不同而表现出不同的光谱特性。进一步研究表明6在不同溶剂中可能以不同的互变异构体存在。     

新型吡唑啉酮衍生物的制备

以氢氧化钾为催化剂,1-苯基-3-甲基-吡唑啉-5-酮与取代苯甲醛亚胺反应合成了新型1-苯基-3-甲基-吡唑啉-5-酮衍生物——1-苯基-3-甲基-4-(1-N-氯乙胺基-1-取代苯基)甲基-吡唑啉-5-酮,其结构经1H NMR,IR,MS和元素分析表征。     

新型含吡唑基的查尔酮的合成、表征及晶体结构

以2种1-苯基-3-甲基-5-对甲苯氧基-吡唑-4-甲醛为原料, 在强碱条件下与苯乙酮(取代苯乙酮)发生羟醛缩合, 高产率地合成出10种新型含吡唑基的查尔酮. 化合物的结构经元素分析, IR和¹H NMR确认. 并用X射线衍射法测定了化合物4c的晶体结构. 化合物4c属三斜晶系, 空间群P-1, 晶胞参数: a＝1.0225(2) nm, b＝1.4263(3) nm, c＝1.6718(3) nm, α＝110.32(3)°, β＝106.30(3)°, γ＝98.11(3)°, M_r＝428.90, V＝2.1159(7) nm³, D_c＝1.346 Mg/m³, Z＝2, F(000)＝896.     

酰基吡唑啉酮缩氨基硫脲Ni(Ⅱ),Co(Ⅲ)和Cr(Ⅲ)配合物的合成、表征及生物活性

合成了含硫席夫碱1-苯基-3-甲基-4-(α-呋喃甲酰基)吡唑啉酮-5缩氨基硫脲(HL)及其Ni(Ⅱ),Co(Ⅲ)和Cr(Ⅲ)配合物.元素分析及摩尔电导率表明,新配合物的组成为[NiL2]·C2H5OH,[CoL2]Cl·H2O,[CrL2]Cl·1/2H2O.运用红外光谱、紫外光谱、核磁共振谱和磁矩对配合物进行了表征.抗菌实验表明,配合物具有较强的抗菌生物活性.     

Crystal Structure and Photochromism in Paint and Solutions of 2,2-Dithiophene-naphthopyran

The title compound 2,2-dithiophene-naphthopyran （C21H14OS2, Mr = 346.44） was synthesized and characterized by IR,^1lH NMR, elemental analysis and single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/n, with a = 8.2349（14）, b = 6.1964（11）, c = 32.458（5）A, β= 95.051（3）°, V= 1649.8（5）A^3, Z = 4, Dc = 1.395 g/cm^3,μ = 0.327 cm^-1, F（000） = 720, the final R = 0.0559 and wR = 0.1442 for 3370 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the interatomic distance of C（13）-O（1） is 1.456（3）A, longer than that of normal C-O bond （1.41 - 1.43 A） in a six-membered heterocycle. The UV-vis spectra of the title compound showed that it exhibits excellent photochromic property in polyester coating and solutions.     

黄连素-染料木素有机盐水合物的制备、晶体结构及溶解性

合成了黄连素和染料木素的有机盐水合物[C₂₀H₁₈NO₄]⁺·[C₁₅H₉O₅]^-·2.5H₂O·0.5(C₂H₅OH),并测定了其晶体结构。 解析结果表明,该有机盐水合物属于单斜晶系,P2₁/c空间群。 染料木素7取代位的羟基失去了质子变成了染料木素阴离子。 羟基阴离子与4'取代位上的羟基形成了O—H••••O^-氢键,产生了一维的氢键链状结构。 两个水分子通过氢键作用形成了链状结构,并与染料木素阴离子形成二维的氢键结构。 加热失去水分子后,有机盐水合物变成无定型状态。 在乙醇水溶液中悬浮后,无定型可以转变成结晶的水合物结构。 形成黄连素-染料木素有机盐水合物后,染料木素在水中的溶解度略有增加。     

Room-Temperature Phosphorescence Invoked Through Norbornyl-Driven Intermolecular Interaction Intensification with Anomalous Reversible Solid-State Photochromism

Herein, norbornyl (NB), a bulky annular nonconjugated spacer, is melded into π systems to construct two groups of ladder-type room-temperature phosphorescence (RTP) luminogens. The effect of the NB on π-π interactions, packing modes and RTP performance is explored systematically. The experimental and computational results demonstrate the versatility of NB in reducing π-π distances and synergistically intensifying the intermolecular interactions, which not only induces intersystem crossing from S₁ to T_n but also diminishes the nonradiative decay of triplet excitons. Impressively, 1800-fold phosphorescence lifetime enhancement is achieved in comparison with the reference compounds without NB. The molecular packing and RTP performance can be further modulated by the length of the backbones and terminal end-groups. It is quite peculiar that NB-annulated phthalic acid exhibits reversible photochromism in the solid state, likely due to the formation of persistent radical pairs. Our study paves an ingenious avenue towards enhancing intermolecular interactions and provides significant implications for a better comprehensive understanding of the origin of their RTP and the inherent photophysical mechanism.     

苯三甲酸-水分子为主体晶格的四丁基铵层状包合物的合成与晶体结构

合成了一种新颖的苯三甲酸 -水分子为主体晶格的四丁基铵氢键包合物 ,(C4H9) 4 N+ [1,3 ,5 C6H3 (COOH) 2 (COO-) ]·2H2 O ,并进行了X射线晶体结构分析 .晶体为单斜晶系 ,P2 1 /c空间群 ,a =1 3 62 1( 2 )nm ,b =1 3 691( 2 )nm ,c =1 60 94( 2 )nm ,β =10 9 665 ( 3 )° ,V =2 82 61( 7)nm3 ,Z =4,R1 =0 0 5 0 8,wR =0 12 17.包合物中 ,苯三甲酸阴离子之间通过 3位与 5位羧基形成的O—H…O分子间氢键键连成沿b轴无限延伸的锯齿形长链 .位于长链较大空隙处的单一氢键键连的水分子二聚体 ,同时与两酸根的羧基生成给体氢键 ,形成一条苯三甲酸阴离子 -水分子复合宽带 .位于宽带外侧的 1位羧基与相邻宽带的水分子生成的氢键 ,将这些宽带连成平行于 ( 0 0 1)面的层状氢键主体晶格 .四丁基铵阳离子层填充在相邻主体晶格的层间空隙处 ,构成“三明治”式夹层结构的包合物     

Synthesis and Properties of a Novel Photochromic Compound

A new photochromic compound containing pyrazolone-ring was synthesized, and its crystal structure was determined on X-ray singlecrystal diffraction, which belongs to monoclinic crystal system, space group P21/c. The UV spectrum of the compound is studied.     

Solid‐State Photochromic Behavior and Thermal Bleaching Kinetics of Two Novel Pyrazolone Phenylsemicarbazones

Two novel photochromic compounds, 1,3‐diphenyl‐4‐benzal‐5‐hydroxypyrazole 4‐phenylsemicarbazone ( 1 a ) and 1,3‐diphenyl‐4‐(4‐nitrobenzal)‐5‐hydroxypyrazole 4‐phenylsemicarbazone ( 2 a ), are synthesized and characterized by elemental analysis, mass spectrometry, FTIR spectroscopy, and ¹H NMR spectroscopy. Their properties, including photochromic behavior, fluorescence properties, and thermal bleaching kinetics, are investigated. The results show that the two compounds exhibit improved photochromic performance in coloration and thermal bleaching rates, excellent photostability, high fatigue resistance, and reversible fluorescence switching properties in the solid state in comparison to reported pyrazolone thiosemicarbazones. The thermal bleaching process obeys first‐order kinetics. Bleaching of powders at 130 °C is completed within 90 s for 1 b (the colored isomer of 1 a ) and 150 s for 2 b (the colored isomer of 2 a ). The activation energy for the thermal bleaching process is determined to be 69 and 95 kJ mol^?1, with frequency factors of 9.5×10⁷ and 9.4×10¹⁰ s^?1 for 1 b and 2 b , respectively.     

Ring-opened Crystal Structure and Photochromism of 2,2-Bis（4-tertiary butyl phenyl）-3H-naphtho[2,1-b]pyran

The title compound, 2,2-bis（4-tertial butyl phenyl） naphthopyran, has been prepared and characterized by means of IR, ^1H NMR and elemental analysis, and its crystal structure was determined with X-ray diffraction in the ring-opened form after hydrolyzation. It belongs to monoclinic, space group P21/c, with a = 14.358（3）, b = 7.6725（15）, c = 24.470（5） А, β= 97.147（4）°, C_33H_36O2, Mr=464.62, V= 2674.8（9）А^3, Z = 4, Dc = 1.154 g/cm^3,μ= 0.070 mm^-1, F（000） = 1000, the final R = 0.0514 and wR = 0.1272 for 5444 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the C（13）-O（1） bond of the title compound cracks after UV irradiation, the six-membered heterocycles are destroyed, and zwitterionic intermediates come into being. The molecular structure in the ring-opened form is obtained after hydrolyzation. It is infrequent that the single-crystal structure is determined in a ring-opened form. A two-dimensional framework is formed by O-H…O and CAr-H…O hydrogen bonds. The UV-vis spectra show that the title compound exhibits excellent photochromic properties in solutions and polymers.     

新型有机磷化合物的合成及其晶体结构

二(三甲基硅基)甲基锂与二甲基胺基腈反应后再与氯代二苯基膦完成膦基取代合成了新型有机磷化合物--(1E,3E)-N1,N1,N3,N3-四甲基-N1′,N3′,2-三(二苯基膦基)丙二酰亚胺(3),其结构经1H NMR,元素分析和XRD表征.3属于正交晶系,Pna2(1)空间群,晶胞参数a=17.265(5)(A),b=8.735 (3)(A),c=29.191(9)(A),α=90.00°,β=90.00°,γ=90.00°,DC=1.175 g·cm-3,Z=4,F(000)=1648.初步探讨了合成3的反应机理.     

萘氧基萘并萘醌的合成和光致变色性质

萘氧基萘并萘醌的合成和光致变色性质方政，杨志范，王淑芝，徐素贤，方天如，王佛松（吉林工学院化工系长春）（中国科学院长春应用化学研究所长春１３００２２）关键词萘氧基萘并萘醌，合成，光致变色苯氧基萘并萘醌类光致变色材料具有耐疲劳，室温下几乎无热消失反应，...     

六芳基二咪唑类化合物的合成及光致变色性能

六芳基咪唑;六芳基二咪唑类化合物的合成及光致变色性能