Daturacin, a new withanolide from Datura innoxia

The methanolic extract of the aerial parts of Datura innoxia afforded a new withanolide, daturacin, the structure of which was elucidated as (20R, 22S)-21,24-epoxy-1,6-dioxo-14alpha-methoxy-5beta-witha-2,25(27)-dienolide (1) by an analysis of the spectroscopic data, including extensive NMR experiments.     

Isolation and structure determination of a benzofuran and a bis-nor-isoprenoid from Aspergillus niger grown on the water soluble fraction of Morinda citrifolia Linn. leaves

The leaves of Morinda citrifolia, Linn. afforded a new benzofuran and a bis-nor-isoprenoid, blumenol C, hitherto unreported from this source. The structures of these have been elucidated as 5-benzofuran carboxylic acid-6-formyl methyl ester (1) and 4-(3'(R)-hydroxybutyl)-3,5,5, trimethyl-cyclohex-2-en-1-one (2) respectively through spectroscopic studies. The NMR data (including 1D, 2D techniques) and stereochemistry at C-3' of Compound 2 is also being reported for the first time.     

Rate Optimality of Wavelet Series Approximations of Fractional Brownian Motion

Consider the fractional Brownian motion process $B_H(t), t\in [0,T]$, with parameter $H\in (0,1)$. Meyer, Sellan and Taqqu have developed several random wavelet representations for $B_H(t)$, of the form $\sum_{k=0}^\infty U_k(t)\epsilon_k$ where $\epsilon_k$ are Gaussian random variables and where the functions $U_k$ are not random. Based on the results of Kühn and Linde, we say that the approximation $\sum_{k=0}^n U_k(t)\epsilon_k$ of $B_H(t)$ is optimal if $$ \displaystyle \left( E \sup_{t\in [0,T]} \left| \sum_{k=n}^\infty U_k(t) \epsilon_k\right|^2 \right)^{1/2} =O \left( n^{-H} (1+\log n)^{1/2} \right), $$ as $n\rightarrow\infty$. We show that the random wavelet representations given in Meyer, Sellan and Taqqu are optimal.     

MEKC determination of vanadium from mineral ore and crude petroleum oil samples using precapillary chelation with bis(salicylaldehyde)tetramethyl‐ethylenediimine

An analytical procedure has been developed for the separation of Cu(II), Ni(II), Co(II), Fe(II), Pd(II), Th(IV), V(IV), and determination of Fe(II), Co(II), Ni(II), and V(IV) by MEKC after chelation with bis(salicylaldehyde)tetramethylethylenediimine (H₂SA₂Ten). Uncoated fused silica capillary was used with an applied voltage of 30 kV with photo‐diode array detection at 228 nm. SDS was added as micellar medium at pH 8.2 with sodium tetraborate buffer (0.1 M). Linear calibrations were established within 0.015–1000 μg/mL of each element with LOD within 5–67 ng/mL. The method was applied for the determination of vanadium from crude oil and ore samples in the range 0.34–2.40 and 114.2–720.7 μg/g with RSD 1.7–3.8 and 0.98–2.30% (n = 3), respectively. Fe, Ni, and Co present in crude oil and ore samples were also determined with RSD 1.3–2.8, 1.1–4.1, and 1.2–3.5% (n = 3), respectively. The results were compared with that of supplier's specifications and atomic absorption spectrometry (AAS). Method was evaluated by standard addition technique.     

Selective monotetrahydropyranylation of symmetrical diols using P_20_5/Si0_2 under solvent-free conditions and their depyranylation

Selective protection of one of the hydroxyl group in 1,n-symmetrical diols is achieved by P_2O_2/SiO_2-catalyzed reaction of the diol with dihydropyran under solvent-free conditions at room temperature.This selective protection is simple and it occurred under economically cheap conditions in high yield.The deprotected diol is simply obtained by refluxing of this compound in methanol using the same catalyst without any byproduct formation or additional purifications.     

Structure determination of salisomide and salisoflavan,two new secondary metabolites from Salsola imbricata,by 1D and 2D NMR spectroscopy

Chromatographic analysis of the alcoholic extract from Salsola imbricata yielded two new secondary metabolites, salisomide (1) and salisoflavan (2). Their structures were established with the help of spectroscopic techniques including COSY, HMQC and HMBC NMR experiments. Copyright © 2008 John Wiley & Sons, Ltd.     

Conversion of iminoacyl quinolinylpalladium (II) complexes into novel oxo‐pyrrolo[3,4‐b] quinolines via depalladation reactions

Oxidative addition reactions of quinolines 1a , b with Pd(dba)₂ in the presence of PPh₃ (1:2) in acetone gave dinuclear palladium complexes [Pd(C,N‐2‐C₉ H₄N‐CHO‐3‐R‐6)Cl(PPh₃)]₂ [(R = H ( 2a ), R = OMe ( 2b ), which were reacted with isocyanide XyNC (Xy = 2,6‐Me₂C₆H₃) to give novel iminoacyl quinolinylpalladium complexes 3a , b in good yields (81 and 77%). Cyclopalladated complexes 3a , b were also obtained in low yields (39 and 33.5%) via one‐pot reaction of 1a , b with isonitrile XyNC:Pd(dba)₂ (4:1). The reaction of 3a , b with Tl(TfO) (TfO = triflate, CF₃SO₃) in the presence of H₂O or EtOH causes depalladation reactions of complexes to provide the corresponding organic compounds 4a , b , 5a , b and 6a , b in yields of 41, 27 and 18 ? 19%, respectively. The products were characterized by satisfactory elemental analyses and spectral studies (IR, ¹H, ¹³C and ³¹P NMR). The crystal structures 2a , 3a and 3b were determined by X‐ray diffraction studies. Copyright © 2008 John Wiley & Sons, Ltd.     

Prediction of hydrogen solubility in heavy hydrocarbons over a range of temperatures and pressures using molecular dynamics simulations

Using the method of molecular dynamics (MD), we have estimated the solubility of hydrogen in heavy hydrocarbons for a range of temperatures and pressures. Heavy hydrocarbon systems are known to be challenging not only for experimental measurements but also for reliable estimations using traditional equations of state (EOS). The simulation system used was designed with semi-permeable membranes to mimic actual experimental studies of gas solubility. Binary interaction parameters between the solute gas and the solvent (heavy hydrocarbons) components were adjusted when necessary to improve agreement with experimental results and then used in subsequent multi-component studies. Temperature and pressure ranges studied included higher temperatures and pressures which are especially difficult to investigate experimentally. Simulation results were finally used to adjust the binary interaction parameters (BIP) in simulation packages (e.g. Aspen) to enable quick and reliable predictions.     

甲烷氧化偶联锂/氧化镁催化剂和纳米催化剂

采用初湿浸渍和溶胶凝胶法分别制备了Li/MgO催化剂和Li/MgO纳米催化剂. 比较两种Li/MgO催化剂对于甲烷氧化偶联反应的催化性能. 采用X射线衍射、BET吸附和透射电镜进行了表征.在973-1073 K和总压力为101 kPa下对催化剂进行了测试. 实验结果表明,Li/MgO纳米催化剂比普通催化剂对于甲烷氧化偶联反应表现为更高的甲烷转换率,较高选择性和较高的的主要产品(乙烷和乙烯)的产率.     

The characterization of soils, clays, and clay firing products

Mössbauer spectroscopic studies of soils are generally centered around the characterization of Fe³⁺ oxides, making use of distinctive magnetic properties of the different oxides and the high sensitivity of the technique for magnetically ordered phases. Most work on clays and clay minerals, in contrast, focuses on the determination of the oxidation state of iron, iron structural site occupancies and distortions, and the transformations that take place during clay firing.