Synthesis and spectral properties of 4-(ortho-R-benzylideneamine)-5-[2-(2-pyridyl)ethenyl]-3-methylisoxazole

The preparation of several 5,4-disubstituted 3-methylisoxazoles is described. The structure of all products was corroborated by ir, ¹H-nmr and mass spectrometry.     

2,5-二甲氧基-4-[(1E)-2-(1H-苯并咪唑-2-基)乙烯基]苯甲醛的合成

以2-甲基苯并咪唑(1)和2,5-二甲氧基-1,4-对苯二甲醛(3)为原料,经缩合反应合成了新化合物——2,5-二甲氧基-4-[(1E) -2-( 1H-苯并咪唑-2-基)乙烯基]苯甲醛(4),其结构经1H NMR,IR和ESI-MS表征.较佳缩合反应条件为:1 11 mol,n(1)∶n(3)=1.1∶1.0,回流反应6h,收率75.2％.     

Thermochromism of 1, 4-Bis[2-(4-pyridyl)ethenyl]-benzene Derivatives

Three kinds of thermochromic materials (DC8, DC12, DC16) were synthesized by linking the rigid 1, 4-bis[2-(4-pyridyl)ethenyl]-benzene (bpeb) with different lengths of alkyl chains. They exhibit remarkable fluorescent color changes under the irradiation of 365 nm light with elevating temperature, which is supposed to be caused by the transition between the crystal state and the amorphous state. Interestingly, the DC16 solid also has a photochromic character. It should be noticed that the phase transition temperatures of three materials measured by differential scanning calorimetry are higher than those of the fluorescence color changes during the heating process. Thus, the allochroic effect is attributed to the synergistic effect of both heating and photo-inducement (365 nm). Ethanol can turn the heated powder into the initial crystal again which indicates that their thermochromic behavior is reversible and makes the fluorescence recover.     

Synthesis of 1,2-dihydroxyindolizidines from 1-(2-pyridyl)-2-propen-1-ol

1-(2-Pyridyl)-2-propen-1-ol, obtained by vinylation of commercially available picolinaldehyde, resulted a good starting material for the synthesis of the indolizidine skeleton. In particular, a simple process involving bromination, reduction, and nucleophilic substitution (via elimination and addition) allowed an easy conversion of the starting material into (±)-lentiginosine in ~27% overall yield.     

Synthesis and crystal structure of (E)-[(2-cyclohexenyl) vinyl]triaryltin

(E)-[(2-Cyclohexenyl)vinyl]triaryltin (aryl=phenyl, p-tolyl) were synthesized and characterized by elemental analysis, IR, 1H NMR spectroscopy. The crystal structure of (E)-[(2-cyclohexenyl)vinyl]triphenyltin was also determined by the X-ray diffraction. Experiments show that this compound has the conjugated system, which makes it have possible bioactivity and anti-tumor activity.     

Synthesis and crystal structure of (E)-[(2-cyclohexenyl)vinyl]triaryitin

(E)-[(2-Cyclohexenyl)vinyl]triaryitin (aryl=phenyl, p-tolyl) were synthesized and characterized by elemental analysis, IR, ¹H NMR spectroscopy. The crystal structure of (E-)[(2 cyclohexenyl)vinyl]triphenyltin was also determined by the X-ray diffraction. Experiments show that this compound has the conjugated system, which makes it have possible bioactivity and antitumor activity.     

4,4′-[1,n-亚烷基双[(E)-2-(4-氧苯基)乙烯基]]双吡啶的光化学性质

通过E-[4-[2-(4-羟基苯基)乙烯基]吡啶与1,n-二溴烷烃亲核取代反应合成了4,4′-[1,n-亚烷基双[(E)-2-(4-氧苯基)乙烯基]]双吡啶[n=2(Ia),3(Ib),4(Ic),6(Id)].用元素分析、红外、紫外和质子核磁共振谱鉴定了Ia～Id的结构.将Ia～Id的稀溶液用中压汞灯和低压汞灯交替照射,发现其分子内光环加成反应的存在,并且随着亚烷基碳链的延长,反应速度加快.研究还发现锌离子可以与吡啶环上氮原子发生螯合作用使分子内光环加成反应加快.本文化合物荧光很弱,在较高浓度下有较强分子间激基缔合物荧光.     

Synthesis, IR spectra, crystal structure and DFT studies on 1-acetyl-3-(4-chlorophenyl)-5-(4-methylphenyl)-2-pyrazoline

1-Acetyl-3-(4-chlorophenyl)-5-(4-methylphenyl)-2-pyrazoline has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction. Density functional (DFT) calculations have been carried out for the title compound by using the B3LYP method at the 6-311G** basis set level. The calculated results show that the predicted geometry can reproduce well the structural parameters. Predicted vibrational frequencies have been assigned and compared with experimental IR spectra and they are supported each other. On the basis of vibrational analyses, the thermodynamic properties of the title compound at different temperatures have been calculated, revealing the correlations between C(0)(p, m), S(0)(m), H(0)(m) and temperatures.     

新型1-吡啶基-3,5-二甲基-1-氢吡唑类化合物的合成及晶体结构

以卤代吡啶为起始原料与水合肼反应合成肼基吡啶衍生物中间体,该中间体进一步与2,4-戊二酮关环合成了一类新型1-吡啶基-3,5-二甲基吡唑衍生物。对合成目标化合物进行了质谱、核磁表征。并且采用X射线单晶衍射分析方法进一步测定了目标化合物1-(3,5,6-三氯吡啶-2-基)-3,5-二甲基-1氢吡唑(3f)的晶体结构。     

5-(3-吡啶基)-2-芳氧乙酰胺基-1,3,4-噻二唑的合成、晶体结构及生物活性

吡啶作为苯环的生物等排体常被用作分子设计的有效基团[1,2],含吡啶类农药已成为近20多年来新农药创制研究的热点领域之一。1,3,4-噻二唑衍生物具有杀虫、杀菌、除草、调节植物生长以及药物活性等多种功效[3-9],因而该类化合物的研究迄今仍方兴未艾。本文根据活性亚结构连接法,     

The crystal and molecular structure of 3,5-Di-(t-butyl)-1-phenylphosphoryl-4-aza-2,5-cyclohexadiene

The crystal and molecular structure of the title compound (C₁₈H₂₆NOP) has been determined by a single crystal, x-ray diffraction study using Cu-Kα. radiation. The compound was found to crystallize in the orthorhombic space group Pnma with unit cell constants a = 12.686 ± .001 Å, b = 14.776 ± .001 Å, and c = 9.540 ± .001 Å. The structure was solved by the heavy atom method and refined by block-diagonal least-squares to a final R = 0.09₉ for the 696 statistically significant reflections. The compound exhibits orientational disorder in the crystalline state. Nevertheless, the planarity of this ring; the lengthening of the diene carbon-carbon bond to 1.41 Å the resultant shortening of both the carbon-nitrogen bond (1.43 Å) and the carbon-phosphorus bond (1.74 Å), and the CNC bond angle of 121° all strongly support the assumption of delocalization of the diene π-electrons within the heterocyclic ring system.     

Synthesis,crystal structure and molecular docking studies of novel 2-(4-(4-substitutedphenylsulfonyl)piperazin-1-yl)quinolone-3-carbaldehyde derivatives

The present work reports the synthesis of novel 2-(4-(4-substitutedphenylsulfonyl) piperazin-1-yl) quinolone-3-carbaldehyde derivatives, namely, 2-(4-tosylpiperazin-1-yl)quinoline-3-carbaldehyde (4a), 2-(4-(4-nitrophenylsulfonyl)piperazin-1-yl)quinoline-3-carbaldehyde (4b) and 2-(4-(4-tert-butylphenylsulfonyl) piperazin-1-yl)quinoline-3-carbaldehyde (4c). These compounds have been characterized by FT-IR, ¹H-NMR, ¹³C-NMR and LCMS. Further, the structures of compounds 4b and 4c have been elucidated by single crystal X-ray diffraction studies. The asymmetric unit of 4b contains two molecules (A and B) and that of 4c contains one. The piperazine ring in both the molecules 4b and 4c has chair conformation and the aldehyde group is twisted with respect to the quinoline group, respectively, by 13.3 (3)°, 18.2 (3)° and 11.2 (3)° in Molecule A & B of 4b and 4c due to the bulky piperazinyl group present in the ortho position. The crystal structures of both features interactions of the type C-H…O, C-H…π_aryl and π_aryl… π_aryl, leading to a three-dimensional (3D) supramolecular architecture in 4b and a one-dimensional (1D) architecture in 4c. The various intermolecular interactions exhibited in 4b and 4c are well supported by Hirshfeld surface and fingerprint plots analysis. Further, the three compounds were evaluated for their in-silico antimicrobial activity. In-silico molecular docking studies were carried out in order to know the binding modes of the synthesized compounds with DNA Gyrase A and N-myristoyltranferase as target proteins for antibacterial and antifungal docking studies, respectively.     

顺式和反式-2-氨基-3-氰基-4-苯基-1-(4'-甲基苯基)-2-环戊烯-1-醇的合成和晶体结构

用低价钛试剂(TiCl4-Zn)与4, 4-二氰基-3-苯基-1-(4'-甲基苯基)-1-丁酮反应合成了顺式和反式-2-氨基-3-氰基-4-苯基-1-(4'-甲基苯基)-2-环戊烯-1-醇, 并用X射线衍射分析确定了这两个异构体的构型。     

Synthesis,polarography and herbicidal activity of quaternary salts of 2-(4-pyridyl)-1,3,5-triazines, 5-(4-pyridyl)pyrimidine, 2-(4-pyridyl)pyrimidine and related compounds

2-(4-Pyridyl)-1,3,5-triazine, 2-(4-pyridyl)-4-methyl-1,3,5-triazine, 2-(4-pyridyl)-4,6-dimethyl-1,3,5-triazine and 2-(4-pyridyl)pyrimidine have been prepared by modification of established triazine and pyrimidine syntheses. These compounds and some of their relatives have been converted to quaternary pyridinium salts. The polarographic reduction potentials of the salts in aqueous solution are pH dependent. The activity of the salts as post-emergent herbicides is reported.     

Synthesis,crystal structure,Hirshfeld surfaces,and spectral properties of Cu(II) and Co(II) complexes with 3-phenoxymethyl-4-phenyl-5-(2-pyridyl)-1,2,4-triazole

A new asymmetrical substituted triazole, 3-phenoxymethyl-4-phenyl-5-(2-pyridyl)-1,2,4-triazole (L) and its complexes, cis-[Cu₂ L ₂Cl₄]·2CH₃CN (1) and trans-[CoL ₂Cl₂]·2H₂O·2CH₃CN (2), have been synthesized and characterized by IR, single-crystal X-ray diffraction, thermogravimetric analyses and Hirshfeld surfaces. In the structure, two L are mainly stabilized by an intermolecular C–H?N hydrogen bond. In 1 (or 2), each L involves a doubly-bidentate (or chelating bidentate) coordination mode through one pyridine and two nitrogens (or one) of triazole, respectively. Complex 1 has a distorted trigonal bipyramidal [CuN₃Cl₂] core with two cis Cl^? while 2 shows a distorted octahedron [CoN₄Cl₂] with two trans Cl^?. We also prepared molecular Hirshfeld surface and fingerprint plot for L, 1 and 2, which revealed the influence of different metals on coordinate of L.     

Sulfanilamide copper(II) chelates with 2-[(2-hydroxyphenyl-imino)methyl]phenolom and 1-[(2-hydroxyphenylimino)-methyl]naphthalen-2-ol

2-[(2-Hydroxyphenylimino)methyl]phenol (H²L¹) and 1-[(2-hydroxyphenylimino)methyl]naphthalen-2-ol (H²L²) reacted with copper(II) acetate hydrate and sulfanilamide (Sf¹), sulfathiazole (Sf²), sulfaethidole (Sf³), sulfadiazine (Sf⁴), and sulfadimidine (Sf⁵) in ethanol to give mixed-ligand copper chelates with the composition Cu(Sf^1–5)(L^1–2) · n H₂O (n = 1, 2). All these complexes are monomeric. Salicylaldehyde imines (H₂L¹ and H₂L²) behave as doubly deprotonated tridentate O,N,O ligands, whereas sulfanilamides (Sf^1–5) are unidentate ligands. Thermolysis of the synthesized complexes includes dehydration at 70–90°C, followed by complete thermal decomposition (290–380°C). The complexes [Cu(Sf¹)(L¹)] · 2H₂O and [Cu(Sf³)(L¹)] · H₂O at a concentration of 10⁻⁴ M inhibited growth and reproduction of 100% of human myeloid leukemia cells (HL-60). The inhibitory effect was 90 and 75%, respectively, at a concentration of 10⁻⁵ M, whereas no antitumor activity was observed at a concentration of 10⁻⁶ M.