Novel 2,6-bis(4-methoxyphenyl)-1-methylpiperidin-4-one oxime esters: synthesis and a new insight into their antioxidant and antimicrobial potential

A simple and efficient protocol for the synthesis of novel 2,6-bis(4-methoxyphenyl)-1-methylpiperidin-4-one oxime esters 4(a-q) is described. Initially, p-anisaldehyde 1 was condensed (Mannich reaction) with acetone and ammonium acetate trihydrate afforded 2,6-bis(4-methoxyphenyl)piperidin-4-one 2. Then, methylation followed by oximation with hydroxylamine hydrochloride (NH(2)OHa (TM) HCl) furnished a key scaffold 4. Further, to explore the enhanced biological properties of the piperidin-4-one core i.e. the key scaffold 4 was conjugated with substituted benzoyl chlorides in the presence of anhydrous K2CO3 as base to obtain novel 2,6-bis(4-methoxyphenyl)-1-methylpiperidin-4-one oxime esters 4(a-q) in excellent yields. The newly synthesized compounds were characterized by elemental analysis, IR, H-1 NMR, C-13 NMR and mass spectroscopic techniques, and screened for their in vitro antioxidant and antimicrobial activities. Most of the compounds exerted positive efficacy towards the biological assays performed. Among the synthesized analogues, compounds 4l and 4m exhibited promising antioxidant activity and on the other hand compounds 4b and 4d manifested persuasive antibacterial activity, whereas compound 4b displayed stupendous antifungal activity against A. flavus strain.

Antiproliferative and tumor inhibitory studies of 2,3 disubstituted 4-thiazolidinone derivatives

4-Thiazolidinone derivatives were synthesized using T3P (R)-DMSO media as a cyclodehydrating agent. All the molecules were tested for their cytotoxicity against leukemic cell lines. The compound 3-(4-bromophenyl)-2-(4-(dimethylamino)phenyl)thiazolidin-4-one (4e) with electron donating substituent at para position of phenyl ring displayed considerable cytotoxicity against Reh and Nalm6 cells with an IC50 value of 11.9 and 13.5 mu M, respectively. Furthermore, the compound 4e tested for tumor regression studies induced by EAC in Swiss albino mouse. Both in vitro and in vivo results suggested significant antiproliferative activity of compound 4e in Reh cells and mouse tumor tissue treated with compound 4e showed multifocal areas of necrosis and numerous number of apoptotic cells. (C) 2015 Elsevier Ltd. All rights reserved.

Spectral characterizations and photophysical properties of one-step synthesized blue fluorescent 4 `-aryl substituted 2,2 `:6 `,2 `'-terpyridine for OLEDs application

We have synthesized a series of 4'-aryl substituted 2,2':6',2 `'-terpyridine (terpy) derivatives, namely 4'-(4-methylphenyl)-2,2':6',2 `'-terpyridine (C-1), 4'-(2-furyl)-2,2':6'2 `'-terpyridine (C-2), and 4'-(3,4,5-trimethoxyphenyl)-2,2':6',2 `'-terpyridine (C-3). The synthesized terpy compounds were characterized by elemental analyses, FTIR, NMR (H-1 and C-13), and ESI-Mass spectrometry. Photophysical, electrochemical and thermal properties of terpy compounds were systematically studied. Maximum excitation band was observed between 240 and 330 nm using UV-visible spectra, and maximum emission peaks from PL spectra were observed at 385, 405 and 440 nm for C-1, C-2 and C-3 respectively. Fluorescence lifetime (tau) of the fluorophores was found to be 035 and 1.55 ns at the excitation wavelength of 406 nm for C-1 and C-2 respectively, and tau value for C-3 was found to be 0.29 ns at the excitation wavelength of 468 nm. We noticed that the calculated values of HOMO energy levels were increased from 5.96 (C-1) to 6.08 (C-3) eV, which confirms that C-3 derivative is more electrons donating in nature. The calculated electrochemical band gaps were 2.95, 2.82 and 3.02 eV for C-1, C-2 and C-3 respectively. These blue fluorescent emitter derivatives can be used as an electron transport and electroluminescent material to design the blue fluorescent organic light emitting diode (OLED) applications. (C) 2015 Elsevier B.V: All rights reserved.

Control of Variable Watermilfoil in Bashan Lake, CT with 2,4-D: Monitoring of Lake and Well Water.

Variable watermilfoil (Myriophyllum heterophyllum Michx.) has recently become a problem in Bashan Lake, East Haddam, CT, USA. By 1998, approximately 4 ha of the 110 ha lake was covered with variable watermilfoil. In 1999, the milfoil was spot treated with Aquacide®, an 18% active ingredient of the sodium salt of 2,4-D [(2,4-dichlorophenoxy) acetic acid], applied at a rate of 114 kg/ha. Aquacide® was used because labeling regarding domestic water intakes and irrigation limitations prevented the use of Navigate® or AquaKleen®, a 19% active ingredient of the butoxyethyl ester of 2,4-D. Variable watermilfoil was partially controlled in shallow protected coves but little control occurred in deeper more exposed locations. 2,4-D levels in the treatment sites were lower than desired and offsite dilution was rapid. In 2000, the United States Environmental Protection Agency (USEPA) issued a special local need (SLN) registration to allow the use of Navigate ® or AquaKleen® in lakes with potable and irrigation water intakes. Navigate® was applied at a rate of 227 kg/ha to the same areas as treated in 1999. An additional 2 ha of variable watermilfoil was treated with Navigate® in 2001, and 0.4 ha was treated in mid-September. Dilution of the 2,4-D ester formulation to untreated areas was slower than with the salt formulation. Concentrations of 2,4-D exceeded 1000 μg/ L in several lake water samples in 2000 but not 2001. Nearly all of the treated variable watermilfoil was controlled in both years. The mid-September treatment appeared as effective as the spring and early summer treatments. Testing of homeowner wells in all 3 years found no detectable levels of 2,4-D.(PDF contains 8 pages.)

Lynx1 and the β2V287L mutation affect the stoichiometry of the α4β2 nicotinic acetylcholine receptor

GPI-anchored neurotoxin-like receptor binding proteins, such as lynx modulators, are topologically positioned to exert pharmacological effects by binding to the extracellular portion of nAChRs. These actions are generally thought to proceed when both lynx and the nAChRs are on the plasma membrane. Here, we demonstrate that lynx1 also exerts effects on α4β2 nAChRs within the endoplasmic reticulum. Lynx affects assembly of nascent α4 and β2 subunits, and alters the stoichiometry of the population that reaches the plasma membrane. Additionally, these data suggest that lynx1 alters nAChR stoichiometry primarily through this intracellular interaction, rather than via effects on plasma membrane nAChRs. To our knowledge, these data represent the first test of the hypothesis that a lynx family member, or indeed any GPI-anchored protein, could act within the cell to alter assembly of multi-subunit protein.

反式和顺式-1，2-二氰-（4-乙基苯）乙烯结构的谱学分析

合成了2种新型的可溶性四氮杂卟啉中间体：反式-1，2二氰-（4-乙基苯）乙烯和顺式-1，2-二氰（4-乙基苯）乙烯。通过UV-Vis，FFIR，GC／MS，^1H NMR等方法对这2种化合物的结构进行了表征，给出了它们完整的结构信息。分析比较了顺、反异构体结构上的差异，分析两者的紫外-可见光谱（UV-Vis）、红外光谱（FTIR）和核磁共振光谱（^1H NMR）谱图的差异及其产生原因。

2,4-D对鱼腥藻增殖的效应

本文在实验室批量培养,室外小池大量培养和塑料大棚大面积培养的基础上,研究了植物激素2,4-D刺激鱼腥藻增殖的效应。浓度在0.01—2.00μg/mL范围内都具有刺激鱼腥藻增殖的效果,随着浓度增加,这种效果降低。品质分析结果表明,0.01μg/mL2.4-D可提高蛋白质和叶绿素a的含量;浓度为0.05μg/mL时,二者的含量与对照相差不大;浓度达到0.1μg/mL时,二者的含量降低。本文提出,2,4-D刺激鱼腥藻增殖的应用浓度应在0.05μg/mL以下,以0.01μg/mL效果最佳。

（一）2，4－二甲基戊二烯基烯土氯化物的合成及其对丁二烯的聚合活性（二）酞菁铜衍生物 LB 膜材料的合成及其气敏特性

本文通过元素分析，红外光谱，热失重分析，质谱。X 光电子能谱的测定以及对化合水解产物的分析。确认合成了下列三种新型 2，4－二甲基戊二烯基稀土氯化物。（I）[2,4-(CH_3)_2C_5H_5]LnCl_2·nTHF (2,4-(CH_3)_2C_5H_5 = 2, 4－二甲基戊二烯基；Ln = Pr, Nd, Sm, Gd; n = 3)。（II）[2,4-(CH_3)_2C_5H_5]LnCl_2·nTHF (Ln = Pr, Nd; n = 2, 3)。（III）[2,4-(CH_3)_2C_5H_5]LnCl_2·nTHF (Ln = Nd, Sm; n = 1)。在稀土金属有机化合物中尚未见此类化合物的报导。化合物的质谱分析结果表明，配位的四氢呋喃分子容易从配合物分子中脱落，形成带一个四氢呋喃，甚至不带四氢呋喃的配合物。说明配合物分子中不带四氢呋喃的形式是较稳定的。化合物的 X 光电子能谱结果表明化合物不是混合物。化合物水解产物的定量气相色谱分析进一步证实所合成的化合物为我们所预期的产物。实验结果表明，单体转化率受溶剂影响较大。在以环戊烷为溶剂的聚合反应中，聚合活性较高。而以甲苯为溶剂的聚合反应中，其聚合活性较低。在主催化剂不变的条件下，改变 Al/Nd 摩尔比，单体的转化率有明显的变化。同一 Al/Nd 摩尔比，不同催化剂用量也对单体的转化率有较大的影响。对聚合物的微观结构分析表明，溶剂，铝钕摩尔比催化剂用量对聚丁二烯的顺－1，4 含量均有影响，但影响不大。

1,2,4-三氯苯胁迫对萌发大豆种子中活性氧的影响

以盆栽法研究了不同浓度 1,2 ,4 三氯苯 (TCB)胁迫对萌发大豆种子中活性氧代谢的影响 .结果表明 ,10 0～ 30 0 μg·g-1TCB胁迫初期 (1～ 3天 )促使萌发大豆种子呼吸强度升高及其峰值提前出现 ,超氧阴离子自由基 (O2 - )及过氧化氢 (H2 O2 )的积累显著增加 ,同时伴随丙二醛 (MDA)含量升高 ,显示发生膜脂质过氧化作用 .TCB胁迫 1～ 6天使活性氧清除酶功能紊乱 ,其中过氧化物酶 (POD)活性升高 ,超氧化物岐化酶 (SOD)活性开始上升后转为下降 .在萌发大豆种子受TCB胁迫伤害过程中 ,活性氧代谢失衡造成的膜脂质过氧化将起着重要作用 .

1，2，4－三氯苯在土壤中的降解

在好氧和厌氧两种条件下研究了１，２，４－三氯苯的降解，结果表明，１，２，４－三氯苯的好氧降解和厌氧降解均遵循一级反应动力学在同样水分、温度及初始浓度条件下，１，２，４－三氯苯的好氧降解比厌氧降解迅速，其半衰期分别为１．８９～５．８６和５．０７～１９．０８ｄ土壤中１，２，４－三氯苯的初始浓度对于其降解也有显著影响，在０～１００μｇ·ｇ－１的范围内，浓度增高时，其降解加快，说明污染物浓度对降解的影响；在１０～３０℃范围内，温度增高导致降解过程加快，归因于温度升高对微生物酶活性的激活作用．

catena-Poly[diammonium [diaquabis(pyridine-2,4-dicarboxylato-kappa N-2,O-2)cuprate(II)] [[diaquacopper(II)]-mu-pyridine-2,4-dicarboxylato-kappa N-3,O-2:O-2 '-[tetraaquacadmium(II)]-mu-pyridine-2,4-dicarboxylato-kappa O-3(2):N,O-2 '] hexahydrate]

The title mixed-metal complex, {(NH4)(2)[Cu(C7H3NO4)(2)(H2O)(2)][CdCu(C7H3NO4)(2)(H2O)(6)]center dot 6H(2)O}(n), contains one octahedrally coordinated Cd-II center and two octahedrally coordinated Cu-II centers, each lying on an inversion center. The two Cu-II atoms are each coordinated by two O atoms and two N atoms from two 2,4-pydc (2,4-H(2)pydc = pyridine-2,4-dicarboxylic acid) ligands in the equatorial plane and two water molecules at the axial sites, thus producing two crystallographically independent [Cu(2,4-pydc)(2)(H2O)(2)](2-) metalloligands. One metalloligand exists as a discrete anion and the other connects the Cd(H2O)(4) units, forming a neutral chain.

Supramolecular isomerism in zinc hydroxide coordination polymers with pyridine-2,4-dicarboxylic acid: Two polymorphs with centrosymmetric two-dimensional and acentric three-dimensional coordination networks

Reactions of Zn(BF4)(2) and pyridine-2,4-dicarboxylic acid (2,4-pydcH(2)) in the presence of 1,2-bis( 4-pyridyl) ethylene or 1,3-bis(4-pyridyl) propane under hydro(solvo) thermal conditions yielded two polymorphic metal-organic coordination polymers formulated as Zn-2(OH)(2)(2,4-pydc) (1 and 2). Polymorph 1 features a two-dimensional (2-D) layer-like structure that is constructed by 2,4-pydc ligands bridging between the Zn-OH-Zn double-chain units. Each single Zn-OH-Zn chain is composed of mu(2)-OH groups connecting trigonal bipyramidal and tetrahedral Zn centers. Polymorph 2 is a 3-D coordination polymer containing 2-D Zn-OH-Zn sheets that consist of mu(2)- and mu(3)-OH groups and trigonal bipyramidal Zn centers. The sheets are pillared by 2,4-pydc ligands to form an acentric structural architecture. 1 and 2 are rare examples that the two polymorphs exhibit a centrosymmetric 2-D coordination network and an acentric 3-D coordination network, respectively. The different structures lead to differences in photoluminescent properties and thermal stabilities for 1 and 2.

catena-Poly[[[di-mu-acetato-kappa O-4 : O '-bis[(acetato-kappa O-2,O ')manganese(II)]]-di-mu-4,4 '-bipyridine-kappa N-4 : N '] monohydrate

The title compound, {[Mn-2(CH3CO2)(4)(C10H8N2)(2)](H2O)-H-.}(n), is a one-dimensional coordination polymer with a ladder-like structure. Two Mn-II atoms, each coordinated by a chelating acetate ligand, are bridged by two bidentate acetate ligands to form a centrosymmetric [Mn-2(CH3CO2)(4)] unit. Two 4,4'-bipyridine ligands link the [Mn-2(CH3CO2)(4)] units through Mn-N bonds to generate a molecular ladder. The water O atom lies on a crystallographic twofold rotation axis.

Crystal structures of EtEDTB center dot 1.4C(2)H(5)OH center dot 5H(2)O and H4EtEDTB(ClO4)(4)center dot C2H5OH (EtEDTB=N, N, N ', N '-tetrakis[2-(1-ethylbenzimidazolyl)methyl]-1,2-ethanediamine)

The crystal structures of EtEDTB.1.4C(2)H(5)OH.5H(2)O 1 and H4EtEDTB(ClO4)(4).C2H5OH 2 (EtEDTB = N, N,N',N'-tetrakis[2-(1-ethylbenzimidazolyl)methyl]-1,2-ethanediamine) have been determined by single-crystal X-ray diffraction method. Compound 1 crystallizes in the space group P(1) over bar with a = 11.489(2), b = 11.866(3), c = 12.002(3) Angstrom, alpha = 97.47(2), beta = 114.564(13), gamma = 114.11(2)degrees, V = 1266.6(5) Angstrom(3), Z = 1, M-r = 847.48, D-c = 1.111 g/cm(3), F(000) = 456 and mu(MoKalpha) = 0.076 mm(-1). A total of 5207 reflections were measured for 1, of which 4323 were independent. The structure of 1 was solved by direct methods and refined by full-matrix least-squares technique to the final R = 0.0706 and wR = 0.1802 for 1318 observed reflections with I > 2sigma(I). In the structure of 1, centrosymmetric EtEDTB molecules are linked by hydrogen bonds through water and ethanol to form 2-dimensional network. Compound 2 crystallizes in the space group C2/c with a = 24.260(5), b = 13.040(3), c = 17.680(4) Angstrom, beta = 97.50(3)degrees, V = 5545.2(2) Angstrom(3), Z = 4, M-r = 1140.80, D-c = 1.366 g/cm(3), F(000) = 2384 and mu(MoKalpha) = 0.289 mm(-1).