bluuebunny/crossref_metadata_2025 huggingface dataset:
Syntheses and crystal structures of [Na(H2O)](C17H13O6SO3)* 2H2O and [NKH2O)6]C17H13O6SO3)2*H2O
Authors: Zhang Zun‐Ting , Guo Ya‐Ning , Liu Qian‐Guang
Published: September 2010

Two hydrates of sodium 5,7‐dihydroxy‐6,4′‐dimethoxyisoflavone‐3′‐sulfonate ([Na(H2O)J(C17H13O6SO3)*2H2O,] 1) and nickel 5,7‐dihydroxy‐6,4′‐dimethoxyisoflavone‐3′‐sulfonate ([Ni(H2O)6](C17H13O6SO3)2*4H2O, 2) were synthesized and characterized by IR, 'H NMR and X‐ray diffraction analyses. The hydrate 1 crystallizes in the mono‐clinic system, space group P2(1) with a=0.8201(9) nm, b=0.8030(8) nm, c= 1.5361(16) nm, β=102.052(12)°, V =0.9893(18) nm3, D,= 1.579 g/cm3, Z=2, μ=0.252 nm−1, F(000)=488, R=0.0353, wR=0.0873. The hydrate 2 belongs to triclinic system, space group P‐1 with a=0.7411(3) nm, b=0.8333(3) nm, c=1.7448(7) nm, α= 86.361(6)°, β=86.389(5)°, γ= 88.999(3)°, V=1.0731(7) nm3, D,=1.587 g/cm3, Z=1, μ=0.649 m−1, F(000)= 534. In the structure of 1, the sodium cation is coordinated by six oxygen atom and two adjacent ones are bridged by three oxygen atoms to form an octahedron chain. The CH…︁… hydrogen bonds exist between two isoflavone molecules in the structure of 2. Meanwhile, hydrogen bonds in two compounds, link themselves to assemble two three‐dimensional network structures, respectively.
Effect of EtOH on the E‐Iodohydroxylation of 1,2‐allenylic sulfoxides with 12
Authors: Fu Chun‐Ling , Chen Guo‐Fei , Deng You‐Qian , Huang Xian , Ma Sheng‐Ming
Published: September 2010

The E‐iodohydroxylation of 1, 2‐allenylic sulfoxides with I2 in the presence of EtOH afforded 3‐phenylsulfinyl‐2–10do‐2(E)‐alkenols in good yields and regio/stereo‐selectivities under very mild conditions.
Synthesis of 2‐Acyl‐2H‐1,2,3‐diazaphospholes and their diels‐alder reaction with cyclopentadiene
Authors: Guo Xiang‐Yun , Wang Quan‐Rui , Tao Feng‐Gang
Published: September 2010

2H‐1,2,3‐Diazaphospholes 3a—3h were prepared from various ketone acylhydrazones and phosphorus trichloride in the presence of triethylamine. Compounds 3 underwent feasible hetero‐Diels‐Alder reactions with cyclopentadiene to afford the respective anellated [1,2,3]diazaphospholes 4a–4d as well as 4a'—d.″ in moderate yields. The endo rule in the reaction was observed under kinetic control conditions.
Efficient and convenient preparation of water‐soluble fullerenol
Authors: Zhang Jian‐Min , Yang Wen , He Ping , Zhu Shi‐Zhengt
Published: September 2010

An efficient and convenient preparation of fullerenols was described. With polyethylene glycol (PEG) 400 as catalyst, fullerenols were conveniently synthesized via the direct reaction of fullerene with aqueous NaOH. By control of reaction conditions, either water‐soluble C, fullerenol or water‐insoluble C60 fullerenol could be obtained selectively.
Reaction of 2,3‐dihydro‐1,5‐benzothiazepines and phenylacetyl chloride in the presence of triethylamine: A new aspect on the formation mechanism of dihydro‐1,3‐oxazin‐4‐one derivatives
Authors: Xu Jia‐Xi , Wang Chao , Zhang Qi‐Han
Published: September 2010

2a,CDisubstituted 2,2a,3,4‐tetrahydro‐2‐phenyl‐1H‐azeto[2,1‐d][1,5]benzothiazepin‐1‐ones, as well as 2‐substituted 2.3‐dihydro‐3‐phenylacetyl‐2‐styryl‐benzothiazoles and 4a,6‐disubstituted 3‐benzyl‐4a,5‐dihydro‐2‐phenyl1‐H,6H‐[1,3]oxazino[2,3‐d][1,5]benzothiazepin‐l‐ones, were obtained from the reaction of 2,4‐disubstituted 2,3dihydro‐1,5‐benzothiazepines with phenylacetyl chloride in the presence of triethylamine. The mechanism for the formation of 4a,5‐dihydro‐1H,6H‐[1,3]oxazino[2,3‐d][1,5]benzothiazepin‐1‐ones, 2,3‐dihydro‐1,3‐oxazin‐4‐one derivatives, was suggested.
Synthesis of an analogue of squalamine: 6β‐hydroxyl‐3‐aminosterol
Authors: Cai Feng , Zhou Wei‐Shan
Published: September 2010

6,β‐Hydroxylsqualamine was synthesized stereoselectively in 13 steps and 19% overall yield from methyl hyodeoxycholanate by using stereospecific epoxidation and asymmetric isopropylation as key steps.
A chiron‐based approach for the synthesis of tricyclic tyrosine analogue
Authors: Liu Fa , Jiao Jiao , Zha Hui‐Yan , Yao Zhu‐Jun
Published: September 2010

A chiron approach‐based enantioselective synthesis of designed tricyclic tyrosine analogue D‐2 was developed. A SmI2‐mediated free radical cyclization, an intramolecular Friedel‐Crafts reaction and an intramolecular Mannich reaction served as key steps. These key steps were optimized and repeated in good yields. All the stereochemistries in the synthesis were established and confirmed.
A novel pentaerythritol‐based carbosilane liquid crystalline dendrimer containing 12 nitroazobenzene groups on the periphery
Authors: Tang Xin‐De , Zhang Qi‐Zhen , Li Ai‐Xiang , Fan Xing‐He , Chen Xiao‐Fang , Zhou Qi‐Feng
Published: September 2010

A novel liquid crystalline dendrimer with peripheral mesogenic units was successfully prepared. Azo‐reaction and Williamson synthesis were employed in the preparation of the mesogenic unit 4–[4–(6‐hydroxyhexyloxy)‐phenylazo]nitrobenzene (M‐NO2). A terminal SiCl functional carbosilane dendrimer based on pentaerythritol was used as dendritic scaffold and subsequently functionalized with the aforementioned groups. Investigation of the liquid crystalline properties of the mesogen‐functionalized dendrimer PCSi‐1G‐NO2 by polarizing optical microscopy, DSC. and X‐ray diffraction showed that it exhibits smectic E (SE) phase, different from the corresponding mesogenic unit, which shows nematic phase. Furthermore. the temperatures of both the melting point and the clearing point of the mesogen‐functionalized dendrimer decrease, and the temperature region of the SE phase is wider than that of the nematic phase.
Supramolecular assemblies of (±)‐2,2′‐Dihydroxy‐1,1′‐binaphthyl with 2,2′‐bipyridine and naphthodiazine
Authors: Ji Bao‐Ming , Chen Hua‐Tng , Du Chen‐Xia , Ding Kui‐Ling
Published: September 2010

Supramolecular assemblies of (±)‐2,2′‐dihydroxy‐1,1′‐binaphthyl (BINOL, A), with aza donor molecules including 2,2′‐bipyridine (B) and naphthodiazine (C), have been synthesized and characterized by single‐crystal X‐ray diffraction methods. Two inclusion complexes crystallize in the triclinic system with P‐1 space group. In the inclusion complex between A and B, two molecules of A and two molecules of B are linked each other by intermolecular hydrogen bonds with two molecules of water as the bridges, forming a centrosymmetric dimer with formula of A2(H2O)2B2; while in the inclusion complex between A and C, the molecule C virtually acts as a bridge to link molecules A through intermolecular OH…︁N hydrogen bonds, forming a short‐chain supramolecular block with a formula of A2'C3 Besides the hydrogen bonding interaction between the host and guest molecules, π‐π stacking interactions also play an important role in the solid‐state packing of these two inclusion complexes. The structural information disclosed on the complex between dihydroxy compound and aza hydrogen bond acceptors in this work would be particularly important for the rational design of supramolecular organic functional materials.
Synthesis and molecular recognition of novel cyclic pseudopeptides containing L‐glutamic acid or L‐aspartic acid backbones
Authors: Wang Tao , Huang Xiao‐Yi , Xia Chuan‐Qin , Yu Xiao‐Qi , Xie Ru‐Gang
Published: September 2010

Novel cyclic pseudopeptides containing L‐glutamic acid or L‐aspartic acid backbone structures were efficiently synthesized and characterized. Their chiral recognition properties for L‐ and D‐amino acid methyl ester hydrochloride were discussed also.
Thermal behavior and decomposition kinetics of the complexes of CuX2 (X=NO3, Br, Cl and ClO4) with 3,3′‐Dimethyl‐1 ‐(1H‐1,2,4‐triazol‐1‐yl)‐2‐butanone
Authors: Lu Zhen‐Rong , Ding Yuan‐Chen , Xu Ying , Li Bao‐Long , Zhang Yong
Published: September 2010

The thermal behaviors of the complexes of CU(DMTZB)4X2 (DMTZB=3,3′‐dimethyl‐1‐(1H‐1,2,4‐triazol‐1‐yl)‐2‐butanone, X=NO3 or ClO4) and CU(DMTZB)2X2 (X=Br or Cl) in a nitrogen atmosphere were studied under the non‐isothermal conditions by simultaneous TG‐DTG‐DSC. EDS and elemental analysis techniques. The results showed that their decomposition proceeded in three different ways mainly depending on the anions in the molecules. The heat effect associated with the decomposition step of DMTZB molecules was also different. The decomposition mechanisms and the kinetic parameters of DMTZB were determined and calculated by jointly using four methods, which showed that its pyrolysis was controlled by D3 mechanism but with different activation energies and pre‐exponential factors for different complexes.
Non‐isothermal kinetics of the decomposition reaction of cluster [Ag3WS3Br](PPh3)3 and [Cu3WS3Br](PPh3)3
Authors: Lu Zhen‐Rong , Ding Yuan‐Chen , Xu Ying , Liu Quan , Lang Jian‐Ping
Published: September 2010

The thermal behaviors of clusters [Ag3WS3Br](PPh3)3 and [Cu3WS3 Br](PPh3)3(PPh3=triphenyl phosphine) in a nitrogen atmosphere were studied under the non‐isothermal conditions by simultaneous TG‐DTG‐DSC and EDS techniques. The results showed that the evolution of PPh3 generally proceeded before the release of the other moiety in one or two step‐mode. The mechanisms, the kinetic and the thermodynamic parameters for decomposition of PPh3 of both clusters were determined and calculated by jointly using several methods, which showed that its evolution was controlled by Avrami‐Erofeev equation. The results also showed that there was no new stable phase composed of W‐Ag(Cu)‐S‐Br after release of organic moiety PPh3 and that CVD method was not applicable to their further processing.
Cation‐π interaction between the aromatic organic counterion and DTAB micelle in mixed solvents
Authors: Deng Dong‐Shun , Li Hao‐Ran , Liu Di‐Xia , Han Shi‐Jun
Published: September 2010

The cation‐π interaction between the aromatic organic counterion potassium hydrogen phthalate (KHP) and DTAB micelle in aqueous mixture of EG was investigated, using the techniques of conductivity measurements, W absorption spectrum and NMR spectrum. The conductivity and UV spectrum studies were with respect to the effect of KHP on DTAB and that of DTAB micelle on KHP, respectively. According to the chemical shift changes of the aromatic ring and the surfactant methylene protons, it can be assumed that KHP penetrated into DTAB micelle with its carboxylic group protruding out of the micellar surface. And the strength of the interaction became weaker with the content of EG in the mixed solvent increasing.
Phase equilibrium system of CsCl‐YCl3‐(9.5%)HCl‐H2O at T=298.15 K and its compounds
Authors: Wang Hui , Duan Jin‐Xia , Ran Xin‐Quan , Gao Shi‐Yang
Published: September 2010

The equilibrium solubility of one CsCl‐YCl3‐H2O ternary section of CsCl‐YCl3‐9.5%HCl‐H2O quaternary system at T=298.15 K was investigated by the physico‐chemical analysis method and the corresponding phase diagram was plotted. The crystallization of two new double salts Cs4YCl7·10H2O (4:1 type) and Cs3Y2Cl9·14H2O (3:2 type) was successful and they were obtained from the complicated system directly. Both were identified and characterized by X‐ray, thermal analysis method of TG‐DTG, DSC. The fluorescence experiments show that up‐conversion phenomenon does not exist in compounds Cs4YCl7·10H2O and Cs3Y2Cl9·14H2O.
Enzymatic synthesis of a CCK‐8 tripeptide fragment
Authors: Xiang Hua , Eckstein Heiner
Published: September 2010

A process for the synthesis of CCK‐8 tripeptide H‐Gly‐Trp‐Met‐OH catalyzed by immobilized enzyme was reported. Enzymes were used for the formation of peptide bonds and the removal of protecting group. starting with phenylacetyl (PhAc) glycin, N‐protected dipeptide PhAc‐Gly‐TrpOMe was obtained by coupling PhAc‐protected glycine carboxamidomethyl ester (Ocam) with Trp‐OMe catalyzed by immobilized papain in buffered ethyl acetate. Then the condensation between PhAc‐Gly‐Trp‐OMe and Met‐OEt·HCl was carried out by immobilized α‐chymotrypsin catalysis in solvent free system. Basic hydrolysis was followed getting PhAc‐Gly‐Trp‐Met‐OH. The PhAc‐group was removed with penicillin G amidase and H‐Gly‐Trp‐Met‐OH was obtained in an overall yield of 43.9%. The reaction conversion of tripeptide in solvent free system was strongly affected by the system of basic salts added. The influence of the support materials used to deposit enzymes and structures of acyl donor and nucleophile on the reaction was also investigated.
Site‐specific deposition of colloidal Pd nanoparticles on self‐assembled microtubules from biolipid
Authors: Fu Yu‐Bin , Zhang Li‐De , Fu Shan‐Gang , Fu Yu‐Bin , Zheng Ji‐Yong
Published: September 2010

Lipid microtubules with wound ribbon features were fabricated by self‐assembling method, and the deposition patterns of colloidal Pd particles on tubular template were investigated. The result indicates that colloidal Pd nanoparticles are preferentially decorated on the helical markings in the interior and on the exterior of preformed tubule and to the edge of loosely helical ribbons to obtain helical deposition features. The multi‐bilayer microstructure of tubules can be marked by fine Pd nanoparticles deposited at the edge of helical ribbon. There are the site‐specific interactions between lipid tubular template and colloidal Pd particles at the helical edge. A new route was illustrated that colloidal Pd particles firmly attach at the edge of thin flat membranes, and then thin membranes roll up and reassemble into tubule together with particles to form helical deposition patterns. The site‐specific deposition of Pd is unbeneficial to obtain the homogeneous metal film on tubules, but it can be utilized to reveal the different chemical nature of lipid molecular assembly.
Electrospray ionization fourier transform ion cyclotron resonance mass spectrometric study on sodium azide cluster ions
Authors: Liu Han‐Qing , Guo Yin‐Long , Lu Hao‐Jie , Chen Guo‐Qiang
Published: September 2010

Sodium aide has rarely been studied in gas phase or in the form of cluster ions and as a model of solid energetic substances and inorganic azide salt was ionized by electrospray ionization (ESI) and studied by high resolution Fourier transform ion cyclotron resonance (FT‐ICR) mass spectrometry (MS) systematically. This paper highlights the effects of experimental conditions on the formation of salt cluster and the collision activation dissociation pathways of cluster ions to develop a microscopic understanding of inorganic azide salt clusters.
Extensive Studies on the AlEt3/THF‐promoted diastereoselective tandem rearrangement/reduction of α‐Hydroxy (amino) heterocyclopropane: An efficient approach to 2‐quaternary 1,3‐diheteroatom units
Authors: Li Xin , Wang Bao‐Min , Zhao Xue‐Zhi , Gao Shuan‐Hu , Tu Yong‐Qiang , Li De‐Run
Published: September 2010

A facile and highly diastereoselective method for the construction of 2‐quaternary 1,3‐amino alcohols and 1,3‐diols has been developed on the basis of the AlEt3/THF‐promoted tandem rearrangement/reductive reaction of α‐hydroxy (amino) aziridines (epoxides). The progressive achievement in this article included that both 2‐epimers of the units could be constructed from the initially same substrate. Also a stereochemistry assignment we reported previously was corrected.
Magnetic field effects on photoreduction reaction of 2‐methyl‐1,4‐naphthoquinone in brij 35 micellar solution with additional radical
Authors: Chen Jia‐Fu , Xue Xuan
Published: September 2010

A study was made of magnetic field effects (MFEs) on the photoreduction reaction of 2‐methyl‐1, 4‐naphthoquinone (MNQ) in Brij 35 micellar solution containing 4‐lauroylamino‐TEMPO (2,2,6,6‐tetramethylpiperidine‐l‐oxyl) radical (L‐R) under magnetic fields below 1.75 T by a nanosecond laser flash photolysis technique. The triplet MNQ mainly underwent the hydrogen abstraction from Brij 35 molecule to give a radical pair. The escaped radical yield increased with magnetic fields from 0 to 0.62 T and then saturated from 0.62 to 1.75 T. MFEs for both system can be explained by the relaxation mechanism. However, it was supposed that additional radical, L‐R affected the MFEs mainly through enhancing the spin‐spin interactions of radical pairs. The effect of the micelle size on MFEs of the studying system was also discussed.
XPS characterization of carbon nanotube supported CoMo hydrodesulfurization catalysts
Authors: Shang Hong‐Yan , Liu Chen‐Guang , Zhao Rui‐Yu , Wu Ming‐Bo , Wei Fei
Published: September 2010

In this paper, the effect of catalytic support and sulfiding method on the chemical state of supported Co‐MO catalysts is studied by XPS. After sulfidation with in‐situ method, the majority of molybdenum in CNT supported CoMo catalyst is transferred to a species with a formal chemical state Mo(IV) in MoS2 phase, and the rest to Mo(V) which consists of Mo coordinated both to O and S, such as MoO2S22‐‐ and MoO3S2‐−. In case of CoMo/γ‐Al2O3 catalyst sulfided with in‐situ method, a fraction of molybdenum is transferred to formal state Moo in the form of MoS2, but there is still a mount of unreduced Mo(VI) phase which is difficult to be sulfided. In CoMo/CNT catalytic system sulfided with ex‐situ method, Mo(IV) in the form of MoS2 is detected along with a portion of unreduced Mo(VI) phase, suggesting that not all the Mo phases are reduced and sulfided by ex‐situ method. As for CoMo/γ‐Al2O3, a portion of molybdenum is sulfided to intermediate reduced state Mo(V) which consists of Mo coordinated both to O and S. such as MoO2S2–2 and MoO3S2–, in addition, there is still a fraction of unreduced Mo(VI) phase. XPS analyses results suggest that CNT support facilitates the reduction and sulfidation of active species to a large extent, and that alumina support strongly interacts with active species, hereby producing a fraction of phase which resists complete sulfiding. Catalytic measurements of catalysts in the HDS of dibenzothiophene (DBT) show that CoMo/CNT catalysts are of higher HDS activity and selectivity than CoMo/γ‐A2O3 catalyst, which is in good relation with the sulfiding behavior of the corresponding catalyst.
Solution‐reaction calorimetric study of coordination compounds of rare earth perchlorates with alanine and imidazole
Authors: Zhao Yan‐Ru , Hou An‐Xin , Dong Jia‐Xin , Zhao Shun‐Sheng , Liu Yi , Qu Song‐Sheng
Published: September 2010

Two coordination compounds of rare earth perchlorates with alanine and imidazole, [RE(Ala)n(Im)(H2O)]‐(ClO4)3(s) (RE=La,n=3; RE=Nd,n=2), have been prepared and characterized. The standard molar enthalpies of reaction for the following two reactions, LaCl3*7H2O(s) + 3Ala(s)+Im(s)+3NaClO4(s)=[La(Ala)3(Im)(H2O)]‐(Cl04)3(S) f 3NaCI(s) + 6H2O(1) (1) and NdCl36H2O(s) + 2Ala(s) + Im(s) + 3NaClO4(s) = [Nd(Ala)2(Im)(H2O)]‐(ClO4)3(s)+3NaCl(s)+5H2O(1) (2), were determined by solution‐reaction calorimetry, at T=298.15 K, as 36.168±0.642 kJ.mol−1and 48.590±0.934 kJ.mol−1respectively. From the results and other auxiliary quantities, the standard molar enthalpies of formation of [La(Ala)3(Im)(H2O)](Cl04)3(s) and [Nd(Ala)2(Im)(H2O)] (Cl04)3(s) were derived, ΔfH{[La(Ala)3(Im)(H2O)](ClO4)3, s) =(−2984.8 ± 1.0) kJ.mol‐land ΔfH{[Nd(Ala)2(Im)(H2O)]‐(ClO4)3,s) =(−2387.8±0.8) kJ.mol−1, respectively.
Synthesis of lanthanide coordination polymers with benzophenone‐4,4′‐dicarboxylate: Effect of lanthanide contraction on structures
Authors: Wang Yi‐Bo , Jin Lin‐Pei
Published: September 2010

Four lanthanide coordination polymers with benzophenone‐4,4′‐dicarboxylic acid (H2bpndc) and 1,10‐phenanthroline (phen), [Ln2(bpndc)3(phen)] (Ln=La (1), Pr (2) and Tb (3)), [Yb(bpndc)15(phen)].05H2O (4) were obtained through solvothermal synthesis. The crystallographic data show that 1, 2, and 3 are isostructural, the Ln(III) ions in 1, 2 and 3 are all eight‐ and ten‐coordinated, respectively, and thus the Ln(III) ions are connected by bpndc ligands, resulting in an interpenetrating 3D structure. While in 4, the Yb(III) ions are eight‐coordinated and connected by bpndc ligands into a 3D structure with 1D rhombic channels, which result from the effect of lanthanide contraction from La(III) to Yb(III) ions, and the bpndc ligands in 1, 2, 3, and 4 display three types of coordination modes.
Synthesis and thermal decomposition mechanism of rare earth (RE=La, Y, Gd) salicylates
Authors: Li Liang‐Chao , Zhou Xiang‐Chun , Zheng Ren‐Wei
Published: September 2010

The rare earth (RE=La, Y, Gd) salicylates were synthesized by the rheological phase reaction method. The complexes were characterized by elemental analysis, infrared spectra (IR), X‐ray powder diffraction (XRD) and thermal gravity analysis (TG). They can be represented by general formula RE(HSal)3 (RE=La, Y, Gd; HSal= C6H4(OH)COO). The crystals of them are monoclinic and have layered structure. The mechanism of thermal decomposition of rare earth salicylates was studied by using TG, DTA, IR and gas chromatography‐mass spectrometry (GC‐MS). The thermal decomposition of the rare earth salicylates in nitrogen gas proceeded in three stages: firstly, they were decomposed to form RE2(Sal)3(Sal=C6H4OCOO) and salicylic acid; then, RE2(Sal)3 were decomposed further to form RE2O(CO3)2 and some organic compounds; finally, RE2O(CO3)2 were decomposed to form rare earth metal oxides (RE2O3) and carbon dioxide. The organic compounds obtained from the second step of the reaction are mainly dibenzofuran, xanthenone, 6H‐benzo[c]chromen‐6‐one, 6‐phenyl‐6H‐benzo[c]chromene, and 1,3‐diphenyl‐1, 3‐dihydro‐2‐benzofuran.
Synthesis, structure and biological activities of novel triazole compounds containing 4,6‐dimethyl‐pyrimidin‐2‐ylthio group
Authors: Xu Liang‐Zhong , Jian Fang‐Fang , Shi Jian‐Gang , Li Lin
Published: September 2010

Four compounds were prepared by reacting 4,6‐dimethyl‐2‐mercaptopyrimidine with a‐bromo‐a‐( 1,2,4‐mazol‐l‐yl)substituted acetylbenzene. Their structures were identified by means of elemental analysis, IR, and 1H NMR spectra. The single crystal structure of 2–[1–(1,2,4triazol‐1‐yl)‐l‐p‐methoxyphenylcarbonylmethylmethylthio]‐4,6‐dimethyl‐pyrimidine was also determined. It crystallizes in monoclinic system, space group P21/c, a=0.8016(2) nm, b=1.2462(3) nm, c= 1.7824(4) nm, β=99.89(3)°, Z=4, V=1.7540(7) nm3, Dc= 1.346 g/cm3, μ=0.205 m‐1, F(000)=744, final R1 =0.0452. There is obviously potentially weak CH…︁N intermolecular interaction between the molecules in the crystal lattice, which stabilizes the crystal structure. The result of the biological test showed that the four compounds all have some fungicidal and plant growth regulating activities.
Study on PEG‐(NH4)2SO4 aqueous two‐phase system and distribution behavior of drugs
Authors: Li Lei , He Chi‐Yang , Li She‐Hong , Liu Feng , Su Shun , Kong Xiang‐Xu , Li Na , Li Ke‐An
Published: September 2010

The distribution behavior of chlorpromazine hydrochloride (CPZ), procaine hydrochloride (PCN) and procaine amide hydrochloride (PCNA) in polyethylene glycol (PEG800 or PEG1500)‐(NH4SO4 aqueous two‐phase systems has been investigated. The result shows that the PEG‐(NH4SO4 aqueous two‐phase system has potential extraction capability in small molecular drug separation. In PEG800–(NH4)2SO4 system, the extraction efficiencies (E) of CPZ, PCN and PCNA amount to 92.8%, 74.5% and 74.4%, respectively, with the distribution coefficients (KD) being 25.7, 5.9 and 5.8, correspondingly. In PEG1500–(NH4)2SO4 system, the extraction efficiencies (E) of CPZ, PCN and PCNA are 93.7%, 71.3% and 63.24, respectively, with distribution coefficients (KD) of 39.6, 6.6 and 5.0, correspondingly. Based on the study on ultraviolet and fluorescence spectra and also distribution behavior of the drugs in PEG‐(NH4)SO4 aqueous two‐phase system, extraction mechanism was further proposed that both hydrogen bond and hydrophobic interaction are involved in extraction.
Near‐infrared hydrophobic probes as molecular light switch for cmc determination of triton X‐100 solution
Authors: Zhu Chang‐Qing , Zheng Hong , Li Dong‐Hui , Li Shun‐Hua , Xu Jin‐Gou
Published: September 2010

The fluorescence behavior of two near‐infrared (NIR) chromophores with linear alkyl chains of different lengths, 2–[4′chloro‐7′(3″ethyl–2″benzothiazolinylidene)‐3′,5′‐(1‴,3‴‐propanediyl)‐1′,3′,5′‐heptantriene‐1′‐yl]‐3‐ethylbenzothiazolium iodide (Robe I) and 2–[4′chloro‐7′(3″hexadecyl‐2″benzothiazolinylidene)‐3′,5′‐(1‴,3‴‐propanediyl)‐1′,3′,5′‐heptantriene‐1′‐yl]‐3‐ethylbenzothiazolium iodide (Probe II), in aqueous solution containing different concentrations of surfactants was studied. The fluorescence of the probe with a short chain (probe I) was completely quenched in water and aqueous solution containing a low concentration (below the critical micelle concentration, CMC) of surfactant Triton X‐100. However, the fluorescence reappeared and reached maximum rapidly once the concentration of the surfactant approached the CMC. The probe with a long chain (probe II) displayed a similar fluorescence behavior but more dramatically fluorescent recovery in Triton X‐100 system, which gave a direct indication for the micelle forming process and provided a simple method for the determination of the critical micelle concentration of the surfactant. The CMC values determined by this method were in good agreement with those obtained by other techniques. The fluorescence behavior of the two probes in other surfactant systems was also investigated.
Chiral borated esters in asymmetric synthesis: 1. the first asymmetric reaction catalyzed by chiral spiroborated esters with an O3BN framework
Authors: Liu De‐Jun , Shan Zi‐Xing , Qin Jin‐Gui
Published: September 2010

The first asymmetric reaction catalyzed by chiral spiroborated esters with an O3BN framework was reported. In the presence of 0.1 equivalent of (R,S)‐1 or (S,S)‐1, acetophenone was reduced by 0.6 equivalent of borne in THF at 0–5 °C for 2 h to give (R)‐1‐phenylethanol of up to 76% ee and 73% isolated yield. Influence of reaction conditions on the stereoselectivity of the reduction was investigated and a possible catalytic mechanism of the chiral spiroborated esters toward the reduction was also suggested.
Gal3 catalyzed tetrahydropyranylation of alcohols and phenols
Authors: Sun Pei‐Pei , Hu Zhi‐Xin
Published: September 2010

In dichloromethane, the nucleophilic addition of alcohols or phenols to 3,4‐dihydro‐2H‐pyran (DHP) was catalyzed effectively by gallium triiodide which was generated in situ by the reaction of gallium metal and iodine to give the corresponding tetrahydropyranyl acetals in good to excellent yields.
Synthesis of the active stilbenoids by photooxidation reaction of trans‐ϵ‐viniferin
Authors: Yao Chun‐Suo , Lin Mao , Wang Ying‐Hong
Published: September 2010

Two new stilbenoids, cis‐ϵ‐viniferin (3) and 2b, 14b‐dehydro‐bisresveratrol (4) were synthesized by photooxidation reaction of trans‐ϵ‐viniferin (2) prepared from tram‐resveratrol (1). Pentamethoxyl trans‐ϵ‐viniferin (5) and pentamethoxyl cis‐ϵ‐viniferin (6) were also obtained by methylation of trans‐ϵ‐viniferin (2) with (MeO)2SO2. Their structures were elucidated on the basis of spectral evidence. Compounds 3 and 4 showed potent inhibition of TNF‐α at concentrations of 10−‐5 mol.L−1 with inhibitory ratios of 51.43% and 36.64%. respectively.
Electrocatalytic oxidation of vitamin B6 by 4‐hydroxy‐2,2,6,6‐tetramethylpiperidine‐N‐oxyl
Authors: Li Yan , Wen Xiao‐Lin , Liu Zhong‐Li
Published: September 2010

The electrochemistry of pyridoxine (vitamin B6, VB6) was studied by cyclic voltammetry at a glassy carbon electrode. The electrochemical response of VB6 could be significantly enhanced by using 4‐hydroxy‐2,2,6,6‐tetra‐methylpiperidine‐N‐oxyl (HO‐TEMPO) as a mediator via an electrocatalytic EC' mechanism with the oxoammonium ion of HO‐TEMPO as the active oxidant. The catalytic rate constant was determined to be 5.4×103 (mol*L−1)−1*s−1 by using chronomperometq.
An efficient synthesis of highly optically active 4‐substituted‐2(5H)‐furanones from chiral 3‐bromo‐2(5H)‐furanone
Authors: Fan Xue‐E , Huang Min , Huang Hui , Chen Qing‐Hua
Published: September 2010

Highly optically active 4‐substituted‐2(5H)‐furanones 6a‐6j were obtained in good yields with de⩾98% by the tandem Michael addition/elimination reaction of chiral 3‐bromo‐2(5H)‐furanone (4a), which was conveniently prepared starting from 2‐furaldehyde under mild conditions. The products were identified on the basis of their satisfactory elemental analysis and spectroscopic data of IR, W, 1H NMR, 13C NMR and mass spectra. The stereochemistry and absolute configuration of this type of compounds were established by the X‐ray crystallographic study. The reaction provided a short and efficient synthesis of the interesting highly optically active 4‐substituted‐2(5H)‐furanones containing an active pyrimidine and a purine base group.
Synthesis of novel carbosilane dendrimers based on pentaerythritol
Authors: Tang Xin‐De , Zhang Qi‐Zhen , Fan Xing‐He , Zhou Qi‐Feng
Published: September 2010

Novel pentaerythritol‐based carbosilane dendrimers centered at carbon have been synthesised. Starting from tetraallyl ether based upon pentaerythrtol as the core molecule, a succession of alternate Pt‐catalyzed hydrosilylation of allyl groups with HSiC13 and allylations of Sicl groups thus introduced with CH2=CHCH2MgBr in THF provided a divergent synthesis of three generations of carbosilane dendrimers in which the Si atoms are linked by CH2CH2CH2 groups. The reaction conditions for hydrosilylation must be well controlled. After purification by chromatography on silica gel pure products for each generation were obtained. The IR, 1H and 13C NMR spectra and elemental analysis data are consistent with the proposed structures. The molecular weights of the resulting carbosilne dendrimers have been determined by vapor pressure osmometry.
Amide‐based fluorescent macrocyclic anion receptors
Authors: Zeng Zhen‐Ya , Xu Kuo‐Xi , He Yong‐Bing , Liu Shun‐Mng , Wu Jin‐Long , Wei Lan‐Hua , Meng Ling‐Zhi
Published: September 2010

Two fluorescent anion receptors (1 and 2) based on amide macrocycle were synthesized and corresponding fluorescence quenching induced by anion complexation was observed in different degree. Receptors form 1:1 complexes with anions by hydrogen bonding interactions. Receptor 1 bound anions in the order of F‐>Cl‐ > H2PO4−‐ CH3COO− > >Br−, I− and receptor 2 showed high selectivity to F− over other anions.
Ab initio calculation of intermolecular dispersion energy and induction energy of nitramide dimer
Authors: Song Hua‐Jie , Xiao He‐Ming , Dong Hai‐Shan , Huang Yi‐Gang , Long Xin‐Ping , Tang Yei‐Peng
Published: September 2010

The dispersion energies, induction energies and their exchange counterparts (exchange‐dispersion and exchange‐induction energies) between two interacting nitramide molecules at several separations are derived based upon symmetry‐adapted perturbation theory (SAPT). The results show that (1) the effect of intramonomer electron correlation on dispersion energies and induction energies for nitramide dimer system is remarkable especially in the region near the van der Waals minimum distance (0.42 nm). (2) At smaller separations the dispersion energies and the induction energies are largely quenched by their exchange counterparts, and this case in induction interaction is much more remarkable than in dispersion interaction. (3) Since at shorter distances there exists the strong short‐range interaction due to electron transfer which quickly decays and even disappears at larger separations, the two different R‐dependency formulae of induction energies were found: one is cu. R−12.7 at short distances, and the other cu R−7.0 at large separations. The latter R‐dependency is similar to that (ca. R−7.2) of dispersion. (4) In the case of strong polar interaction existing in nitramide dimer, the “true” induction correlation terms of higher order than 1Eind(22) may be important.
Direct electrochemistry of cytochrome c on EDTA‐ZrO2 organic‐inorganic hybrid film modified electrodes
Authors: Xu Jing‐Juan , Peng Ying , Liu Shou‐Qing , Chen Hong‐Yuan
Published: September 2010

A composite film of ethylenediamine tetraacetic acid (EDTA)‐ZrO2 organic‐inorganic hybrid was prepared based on the chelation between Zr(IV) and EDTA. The direct electrochemical behavior of cytochrome c (cyt. c) at the hybrid film modified glassy carbon electrodes was investigated. The immobilized EDTA can promote the redox of heme in horse heart cyt. c which gives rise to a pair of reversible redox peaks with a formal potential of 40 mV (vs. SCE). The peak current increased linearly with the increase of cyt. c concentration in the range of 1.6 × 10−6—8.0 × 10−5 mol·L−1 with the correlation coefficient of 0.996. Further investigation shows that metal ions can impede the electron transfer of cyt. c. The impediment capability of metal ions depends on their coordination capability with EDTA and their valence number.
Novel role of carbon dioxide as a selective agent in palladium‐catalyzed cyclotrimerization of alkynes
Authors: Li Jin‐Heng , Xie Ye‐Xiang
Published: September 2010

Carbon dioxide was found as a selective agent to promote the palladium‐catalyzed cyclotrimerization of alkynes in water. Both aryl and alkylacetylenes afforded the corresponding cyclotrimerization products regioselectively in high yields using PdCl2, CuCl2, and CO2 as the catalytic system. However, tert‐butylacetylene bearing a bulky group gave a dimerization product. Mechanism of this reaction was also discussed.
The concentration of hydrogen peroxide generated during aggregation of α‐synuclein in vitro is lower than 5 nmol/L
Authors: Ji Li‐Na , Li Hong‐Tao , Luo Xiao‐Ying , Zhang Feng , Hu Hong‐Yu , Hu Jun
Published: September 2010

Using a fluorometric method with a detection limit of 5 nmol/L. here it is reported that albeit positive results were got from bovine serum albumin (BSA) and chicken ovalbumin (OVA) as published in literature, no detectable amount of hydrogen peroxide (H2O2) was generated during α‐synuclein (α‐Syn) aggregation in vitro even in the presence of transition metal ions Cu(II) or Fe(III). The results suggest that the concentration of H2O2 generated during aggregation of α‐Syn in vitro be lower than 5 nmol/L beyond the detection limit of the adopted method and it is far too poor to be responsible for the cytotoxicity of α‐Syn aggregates, thus allowing people to extensively elucidate the mechanism underlying neurotoxicities of the aggregates formed by some amyloidogenic proteins.
Microcalorimetric studies on influence of Sm3+, Dy3+ on growth and sporulation of Bacillus thuringiensis
Authors: Zhao Ru‐Ming , Liu Yi , Yang Chang‐Ving , Xie Zhi‐Xiong , Shen Ping , Qu Song‐Sheng
Published: September 2010

By using an LKB‐2277 Bioactivity Monitor and cycle‐flow method, the thermogenic curves of aerobic growth for Bacillus thuringiensis cry II strain at 28 °C have been obtained. The metabolic thermogenic curves of Bt cry II contain two distinct parts: the first part reflects the changes of bacterial growth phase and the second part corresponds to sporulation phase. From these thermogenic curves in the absence or presence of Sm3+, Dy3+ ions, the thermokinetic parameters such as the growth rate constants k, the interval time τI, the maximum power PMAX1 and heat‐output QLOG for log phase, the maximum power PMAX2 and heat‐output QSTAT for stationary phase, the heat‐output QSPOR for sporulation phase and total heat effects QT were calculated. Sm3+ and Dy3+ ions have promoting action on the growth of Bt cry II in their lower concentration range, on the other hand, they have inhibitory action on the sporulation of Bt in their higher concentration range. It has also been found that the effects of Sm3+ and Dy3+ ions on Br firing the sporulation phase were far greater than those during the bacterial growth phase. It was concluded that the application of Bt for controlling insecticide could not be affected by the presence of the rare‐earth elements in the environmental ecosystem.
Atmospheric and Surface Water Pollution Interpretation in the Gdańsk Beltway Impact Range by the Use of Multivariate Analysis
Authors: Dubiella‐Jackowska Aleksandra , Astel Aleksander , Polkowska Żaneta , Staszek Wojciech , Kudłak Błażej , Namieśnik Jacek
Published: September 2010

The present study deals with the application of the hierarchical cluster analysis and non‐parametric tests in order to interpret the Gdańsk Beltway impact range. The data set represents concentration values for major inorganic ions (Na+, NH, K+, Mg2+, Ca2+, F−, Cl−, NO, and SO) as well as electrolytic conductivity and pH measured in various water samples [precipitation, throughfall water, road runoff, and surface water (drainage ditches, surface water reservoirs, and spring water)] collected in the vicinity of the beltway. Several similarity groups were discovered both in the objects and in the variables modes according to the water sample. In the majority of cases clear anthropogenic (fertilizers usage and transport, road salting in winter) and semi‐natural (sea salt aerosols, erosion of construction materials) impacts were discovered. Spatial variation was discovered for road runoff samples and samples collected from surface water reservoirs and springs. Surprisingly no clear seasonal variability was discovered for precipitation chemistry, while some evidences for existing of summer and winter specific chemical profile was discovered for road runoff samples. In general, limited range of the Gdańsk Beltway impact was proven.
Malachite Green Adsorption by a Residue‐based Microwave‐activated Adsorbent
Authors: Franca Adriana S. , Oliveira Leandro S. , Nunes Anne A.
Published: September 2010

An adsorbent obtained by microwave activation of defective coffee press cake was evaluated for malachite green (MG) removal from aqueous solutions. Batch adsorption tests were performed and the effects of particle size, contact time, adsorbent dosage, initial solution pH, and initial dye concentration on MG removal from aqueous solutions were investigated. Adsorption kinetics was determined by fitting pseudo‐first‐ and second‐order kinetic models to the experimental data, with the second‐order model providing the best description of MG adsorption onto the prepared adsorbent. The experimental adsorption equilibrium data were better described by the Langmuir model in comparison to Freundlich. The results presented in this study show that the produced adsorbent presents great potential as an inexpensive and easily available alternative for the removal of cationic dyes in wastewater treatments.
Cell type‐dependent biomarker expression in adenoid cystic carcinoma
Authors: Bell Diana , Roberts Dianna , Kies Merrill , Rao Pulivarthi , Weber Randal S. , El‐Naggar Adel K.
Published: September 2010

BACKGROUND:

Adenoid cystic carcinoma (ACC), a rare and progressive salivary malignancy, is characterized by cellular, morphologic, and clinical heterogeneity. The authors of this report hypothesized that the dual cellular composition of ACC plays an important role in biomarker evaluation, tumor biologic behavior, and response to therapy.

METHODS:

To investigate the differential localization and expression of the c‐Kit protein and the epidermal growth factor receptor (EGFR) protein, immunohistochemical analyses were performed on tissue arrays that were constructed from 199 tumors, and the results were correlated with clinicopathologic factors.

RESULTS:

c‐Kit expression was limited to the inner ductal epithelial cells, whereas EGFR expression was limited mainly to the outer myoepithelial cells in the majority of ACCs with tubular and cribriform patterns. In solid ACCs, c‐Kit uniformly was positive, whereas EGFR consistently was negative. A significant statistical correlation was observed between c‐Kit expression and a poor 3‐year outcome, and EGFR expression was correlated with a better 3‐year outcome.

CONCLUSIONS:

The current findings underscored the importance of cellular subtype localization of biomarkers in the clinical and therapeutic stratification of patients with ACC. Cancer 2010. © 2010 American Cancer Society.
Buzzwords on their way to a tipping‐point: A view from the blogosphere
Authors: Neuman Yair , Nave Ophir , Dolev Eran
Published: September 2010

“Buzzwords” are new words (i.e., neologisms) that enter the language and acquire great popularity as “fashion words.” To date, the dynamic aspect of buzzwords has not been the subject of a rigorous scientific analysis. In this study, we analyzed the appearance of buzzwords in the blogosphere and compared their dynamics to the one of nonpopular neologisms and well‐established words. It was found that the growth rate of buzzwords is exponential and higher than that of the blogosphere. Moreover, we have identified general early warning signals for an approaching tipping point in the dynamics of buzzwords indicating that as fashion words they are on their way to a tipping‐point of decline. The article presents these findings and others and concludes by presenting a model for studying the dynamics of new words entering the language. © 2010 Wiley Periodicals, Inc. Complexity 16: 58‐68, 2011
Miniaturizing bromodeoxyuridine incorporation enables the usage of flow cytometry for cell cycle analysis of adherent tissue culture cells for high throughput screening
Authors: Cappella Paolo , Giorgini Maria Laura , Ernestina Re Claudia , Ubezio Paolo , Ciomei Marina , Moll Jürgen
Published: September 2010

Analysis of cell cycle progression by 5‐bromo‐2′‐deoxyuridine (BrdU) incorporation is commonly used for evaluating the mode of action of anticancer drugs, but usually requires a high number of cells and large amounts of monoclonal antibodies. In addition, manual sample handling is not suitable for high throughput. To circumvent these limitations, we have developed a miniaturized method to measure BrdU incorporation into DNA directly in 96‐wells plates. Adherent cells were grown in 96‐well plates in the absence or presence of compounds of interest. After BrdU pulse labeling or pulse chase, cells were harvested, transferred to polymerase chain reaction (PCR) V‐bottom plates, and fixed by adding methanol. DNA denaturation was performed directly in the plates by heat using a PCR thermocycler. BrdU incorporation was detected by indirect immunocytochemical staining, and cellular DNA was counterstained using propidium iodide. Samples were acquired by a BD FACSCalibur with BD Multiwells Auto sampler or BD HTS. We defined a dynamic range of the optimal cell number, for which cells maintained exponential growth up to 72 h. The assay was robust up to 30,000 cells per well. BrdU dot plots of cell cycle phases showed an excellent separation of cell populations, and DNA histograms showed a low coefficient of variation. Thermal denaturation was suitable for 96‐well plates to detect BrdU incorporation with a good signal‐to‐noise ratio, and cluster analysis allowed fingerprint readouts for drug sensitivity and mechanism of action as exemplified for paclitaxel and doxorubicin. This method provided rapid high‐throughput BrdU/DNA content analysis with high accuracy and reproducibility, accompanied by a reduction in reagent consumption. A critical step was identified as the standardization of DNA denaturation using a PCR thermocycler. Here,we show some applications of this method for cell cycle studies in drug discovery. © 2010 International Society for Advancement of Cytometry
Tyramide signal amplification for analysis of kinase activity by intracellular flow cytometry
Authors: Clutter Matthew R. , Heffner Garrett C. , Krutzik Peter O. , Sachen Kacey L. , Nolan Garry P.
Published: September 2010

Intracellular flow cytometry permits quantitation of diverse molecular targets at the single‐cell level. However, limitations in detection sensitivity inherently restrict the method, sometimes resulting in the inability to measure proteins of very low abundance or to differentiate cells expressing subtly different protein concentrations. To improve these measurements, an enzymatic amplification approach called tyramide signal amplification (TSA) was optimized for assessment of intracellular kinase cascades. First, Pacific Blue, Pacific Orange, and Alexa Fluor 488 tyramide reporters were shown to exhibit low nonspecific binding in permeabilized cells. Next, the effects of antibody concentration, tyramide concentration, and reaction time on assay resolution were characterized. Use of optimized TSA resulted in a 10‐fold or greater improvement in measurement resolution of endogenous Erk and Stat cell signaling pathways relative to standard, nonamplified detection. TSA also enhanced assay sensitivity and, in conjunction with fluorescent cell barcoding, improved assay performance according to a metric used to evaluate high‐throughput drug screens. TSA was used to profile Stat1 phosphorylation in primary immune system cells, which revealed heterogeneity in various populations, including CD4+ FoxP3+ regulatory T cells. We anticipate the approach will be broadly applicable to intracellular flow cytometry assays with low signal‐to‐noise ratios. © 2010 International Society for Advancement of Cytometry
Methods of collection of biological information for fatigue evaluation during visual display terminals (VDTs) operation
Authors: Hachiya Yuriko , Ogai Harutoshi , Okazaki Hiroko , Fujisaki Takeshi , Uchida Kazuhiko , Oda Susumu , Wada Futoshi , Mori Koji
Published: September 2010

A method for the analysis of fatigue parameters has been rarely researched in VDT operation. Up to now, fatigue was evaluated by changing of biological information. If signals regarding fatigue are detected, fatigue can be measured. The purpose of this study was an experiment and analysis method to extract parameters related to fatigue from the biological information during VDT operation using Independent Component Analysis (ICA). The experiment had 11 subjects, and examined light‐load and heavy‐load VDT operation. Measurement items were amount of work, number of mistakes, subjective symptoms, surface skin temperature (forehead and apex nasi), heart rate, skin blood flow of forearm, and respiratory rate. In the heavy‐load operation group, number of mistakes and subjective symptom score were increased. Two‐factor ANOVA was used for analysis. The result of number of mistakes was confirmed for the heavy load. After the moving averages of waveform were calculated, we extracted independent components by using ICA. The results of ICA suggest that the independent components increase according to accumulation of fatigue. Thus, the independent components would be a possible parameter of fatigue. However, further experiments should continue in order to obtain conclusive findings of our research. © 2010 Wiley Periodicals, Inc. Electron Comm Jpn, 93(9): 47–57, 2010; Published online in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/ecj.10033
Legibility evaluation with oculomotor analysis. The relationship between contrast and legibility
Authors: Saito Daisuke , Saito Keiichi , Saito Masao
Published: September 2010

Web page legibility is important because of the widespread use of the World Wide Web, and color combinations between the foreground and background are crucial to assuring sufficient legibility. In our previous studies, the visibilities of several web‐safe color combinations were examined using a psychological method. In those studies, simple stimuli were used because of experimental restrictions. In this study, the legibility of sentences on Web sites was examined using an oculomotor‐based psychophysiological method, and the effect of achromatic color combinations, that is, the contrast, was examined in terms of the calculated reading time. The presentation stimuli were positive colorations, whose font color luminance was lower than the background color, and negative colorations, whose font color luminance was higher than the background color. The number of characters per line was arranged to be the same on each page, and four levels of achromatic contrast (the contrast between the background color and the font color), namely, 92.5%, 75.0%, 50.0%, and 25.0%, were examined. It was shown that the reading time increased when the contrast decreased. However, with negative coloration, there were great differences between individuals. Therefore, considering web accessibility, legibility is found to be improved when using a positive coloration. © 2010 Wiley Periodicals, Inc. Electron Comm Jpn, 93(9): 27–33, 2010; Published online in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/ecj.10243