Slow-rise and fast-drop current feature of ultraviolet response spectra for ZnO-nanowire film modulated by water molecules

This study describes the fabrication of ZnO-nanowire films by electro-chemical anodization of Zn foil.The ZnO films are characterized by field emission scanning electron microscopy,X-ray diffraction patterns,and transmission electron microscopy,respectively.The ultraviolet(UV) photo-response properties of the surface-contacted ZnO film are studied through the current evolution processes under different relative humidities.Unlike the usually observed current spectra of the ZnO films,the drop time is shorter than the rise time.The photo-conductivity gain G and the response time τ are both increased with the increase of the applied bias.The photo-conductivity gain G is lowered with the increase of the environmental humidity,while the response time τ is increased.These results can be explained by considering three different surface processes:1) the electron-hole(e-p) pair generation by the UV light illumination,2) the following surface O2-species desorption,and 3) the photo-catalytic hydrolysis of water molecules adsorbed on the ZnO surface.The slow-rise and fast-drop current feature is suggested to originate from the sponge-like structure of the ZnO nanowires.     

KMnO4-mediated direct selective radical cross-coupling: An effective strategy for C2 arylation of quinoline N-oxide with arylboronic acids

Direct C—H functionalization of quinoline N-oxides with arylboronic acids is achieved using KMnO_4 as the sole and efficient oxidative system.This method provides an efficient protocol to construct regioselectively 2-arylquinoline N-oxides via radical cross-coupling reaction in moderated to good yields under mild conditions.     

Cu(OAc)2-catalyzed direct radical C2 arylation of quinoline N-oxide with arylamines

A Cu(OAc)₂-catalyzed synthesis of 2-arylquinoline N-oxides with easily available arylamines is described. The main features of this reaction are mild reaction conditions, high functional-group tolerance, excellent regioselectivity, and good to excellent yields. This procedure is mild, operationally simple, and constitutes a greener approach to the arylation of quinoline N-oxides.     

N-3烷基取代嘧啶及其衍生物的合成

在室温条件下,经过三步反应,合成了一系列N-3烷基取代的嘧啶类化合物.该方法具有条件温和、操作简便、反应时间短、产率高等特点.目标产物经过了1HNMR,13C NMR和MS确证表征.     

Synthesis and Application of N-Tosyl Piperidinyl-Containing α-Aminophosphonates

Abstract

A series of novel (4′-tosyl) piperidin-4-yl containing α-aminophosphonates were synthesized by a one-pot reaction, efficiently catalyzed by magnesium perchlorate, under solvent-free conditions from 1-tosylpiperidin-4-one, substituted aromatic amines, and diethyl phosphite (DEP). The synthesized compounds were characterized by IR, ¹H NMR, ¹³C NMR, ³¹P NMR, and HRMS spectroscopy. A single-crystal X-ray structure of diethyl 4-(2-chlorophenyl) amino-1-(4’-methylbezenesulfonyl) piperidin-4-yl-phosphonate (2a) was obtained, and some of the title compounds displayed insecticidal activities against Plutella xylostella.

Supplementary materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfer, and Silicon and the Related Elements for the following free supplemental files: Additional figures and tables.     

Metal-free synthesis of (E)-vinyl sulfones via denitrative coupling reactions of β-nitrostyrenes with sodium sulfinates

Abstract

A practical metal-free procedure for the synthesis of (E)-vinyl sulfones has been developed through the coupling of β-nitrostyrenes with sodium sulfinates under microwave irradiation. This methodology provides a convenient and efficient approach to various (E)-vinyl sulfones from readily available starting materials with excellent regioselectivity. The present oxidative reaction involves an efficient denitrative radical cross-coupling of β-nitrostyrenes with sodium sulfinates via using AcOH as an additive.     

Comparison of direct mass spectrometry methods for the on‐line analysis of volatile compounds in foods

For the on‐line monitoring of flavour compound release, atmospheric pressure chemical ionization (APCI) and proton transfer reaction (PTR) combined to mass spectrometry (MS) are the most often used ionization technologies. APCI‐MS was questioned for the quantification of volatiles in complex mixtures, but direct comparisons of APCI and PTR techniques applied on the same samples remain scarce. The aim of this work was to compare the potentialities of both techniques for the study of in vitro and in vivo flavour release. Aroma release from flavoured aqueous solutions (in vitro measurements in Teflon bags and glass vials) or flavoured candies (in vivo measurements on six panellists) was studied using APCI‐ and PTR‐MS. Very similar results were obtained with both techniques. Their sensitivities, expressed as limit of detection of 2,5‐dimethylpyrazine, were found equivalent at 12 ng/l air. Analyses of Teflon bag headspace revealed a poor repeatability and important ionization competitions with both APCI‐ and PTR‐MS, particularly between an ester and a secondary alcohol. These phenomena were attributed to dependency on moisture content, gas/liquid volume ratio, proton affinities and product ion distribution, together with inherent drawbacks of Teflon bags (adsorption, condensation of water and polar molecules). Concerning the analyses of vial headspace and in vivo analyses, similar results were obtained with both techniques, revealing no competition phenomena. This study highlighted the equivalent performances of APCI‐MS and PTR‐MS for in vitro and in vivo flavour release investigations and provided useful data on the problematic use of sample bags for headspace analyses. Copyright © 2013 John Wiley & Sons, Ltd.     

Synthesis of symmetrical 1, 3-diynes via tandem reaction of (Z)-arylvinyl bromides in the presence of DBU and CuI

Microwave-assisted tandem reaction of(Z)-arylvinyl bromides involving an elimination and homocoupling in the presence of DBU and Cul in DMF affords a variety of symmetrical 1,3-diynes in good to excellent yields.This tandem process,eliminating the need of volatile and savory terminal alkynes,provides an alternative to the conventional homocoupling methods for the synthesis of symmetrical 1,3-diynes.     

密闭高压消解–ICP–AES测定进口铜精矿中铅、镉、汞、砷

采用密闭高压消解法对样品进行消解,用电感耦合等离子体发射光谱法(ICP–AES)测定进口铜精矿中的铅、镉、砷、汞有害元素。铅、镉、砷、汞的工作曲线分别在0~10,0~1,0~4,0~0.6μg/mL范围内线性良好,线性相关系数大于0.999。各元素加标回收率均为91.0%~104.7%,相对标准偏差均小于3%(n=7)。将密闭高压消解法与电热板加热法和微波消解法进行了比对分析,结果显示,密闭高压消解–ICP–AES法适合用于铜精矿样品的消解与测定。