中国化学快报

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Palladium-catalyzed Cascade Cyclization-Coupling Reaction of Benzyl Halides with N,N-Diallylbenzoylamide

Yi Min HU, Yu ZHANG, Jian Lin HAN, Cheng Jian ZHU, Yi PAN

中国化学快报. 2003, 14(08): 771-772.

摘要 ( )

可视化

A novel type of palladium-catalyzed cascade cyclization-coupling reaction has been found. Reaction of N, N-diallylbenzoylamide 1 with benzyl halides 2 afforded the corresponding dihydropyrroles 3 in moderate to excellent yields.

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Reduction of Azides to Amines with New Metal/Lewis Acid Systems in H₂O or Aqueous EtOH

Chun Bao LI, Peng Wu ZHENG, Zhu Xuan ZHAO, Wen Qin ZHANG, Meng Bao LI, Qi Chao YANG, Yi CUI, Yan Li XU

中国化学快报. 2003, 14(08): 773-775.

摘要 ( )

可视化

The azides were reduced to the corresponding amines by two new metal/Lewis acid systems in water or in aqueous EtOH in yields ranging from 80%-95%. The reaction rates were faster in water than in aqueous EtOH in most cases. All 16 azides with different functional groups were well reduced to the corresponding amines in excellent yields and reaction rates.

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The Synthesis of Glycoglycerolipids

Chun Xia LI, Ying Xia LI, Ling Bo YU, Hua ZHANG, Shi Dong CHU, Hua Shi GUAN

中国化学快报. 2003, 14(08): 776-778.

摘要 ( )

可视化

A convenient synthetic route was developed for the synthesis of the novel glycolipids:1, 2-di-O-acyl-3-O-(2'-acylamide-2'-deoxy-α-D-glucopyranosyl)-sn-glycerols. 10 new compounds of glycolipids with different acyl groups were obtained.

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Synthesis and Chiral Separation of Dinucleotide (TpAZT) Phosphoramidates

Chang Xue LIN, Hua FU, Guang Zhong TU, Yu Fen ZHAO

中国化学快报. 2003, 14(08): 779-782.

摘要 ( )

可视化

Dinucleotide (TpAZT) phosphoramidates were synthesized by Todd reaction of dinucleoside H-phosphonates and amino acid methyl esters, and their diastereomers (R_p and S_p) were separated by crystallization, and the results showed that natural and cheap methyl esters of alanine and phenylalanine can be used for large-scale synthesis of dinucleotide analogs.

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Synthesis of Coronene Using Microwave Irradiation

Bing YANG, Ying LI, Ming Gui XIE

中国化学快报. 2003, 14(08): 783-785.

摘要 ( )

可视化

Using microwave irradiation, perylene was obtained from 3,4,9,10-perylenetetracar-boxylic dianhydride with copper powder in boiling quinoline. With the same method, 1,12-benzoperylene was synthesized from 1,12-benzoperylene-1',2'-dicarboxylic anhydride, and coronene was prepared from coronene-1,2-dicarboxylic anhydride with good yield. Through Dields-Alder reaction, 1,12-benzoperylene-1',2'-dicarboxylic anhydride and coronene-1,2-dicarboxylic anhydride were also prepared using microwave irradiation.

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Synthesis and Selective Coloration of Monoaza Crown Ethers Bearing Picrylamino-type Side Arms for Alkali Metal Salts and Methylamine

Wei ZENG, Zhi Hua MAO, Mi GONG, Chun Chun ZHANG, Sheng Ying QIN, Jun SU

中国化学快报. 2003, 14(08): 786-789.

摘要 ( )

可视化

N-pivot lariat ethers with picrylamino group as a chromophore (1, 2 and 3) have been prepared by reaction of N-(4-aminoaryl)monoaza crown ethers with picryl chrolide, and the selective coloration of 1, 2 and 3 for alkali metal salts and amines has been studied by UV-Vis spectra.

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Synthesis of 4-Amino-5-furyl-2-yl-4H-1,2,4-triazole-3-thiol Derivatives as a Novel Class of Endothelin (ET) Receptor Antagonists

Xin Yong LIU, Wen Fang XU, Jing De WU

中国化学快报. 2003, 14(08): 790-793.

摘要 ( )

可视化

A series of novel 3-alkylthio-4-arylideneamino-5-(2-furyl)-1,2,4-triazole derivatives were synthesized. Their chemical structures were confirmed with elemental analysis and spectral data. Endothelin(ET) receptor competitive binding assay showed that some compounds exhibited high selective as potent ET-1 receptor antagonist.

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Preparation of Molecular Imprinted Copolymer Membrane for Uracil Recognition

Shao Ling XIA, Hong Ying WANG, Hong SUN, Yu Kun LIU, Shao Kui CAO

中国化学快报. 2003, 14(08): 794-796.

摘要 ( )

可视化

Uracil molecular imprinted membrane was prepared by phase inversion technique with[P(AN-co-MAA)] copolymer. SEM photograph shows that the resultant membrane has a typical ultrafiltration structure with Water Volume Flux of 3.7×10^-5m³/m²·s, and uracil substrate permeation experiment shows that the resultant membrane can bind uracil into its structure, and shows a binding equilibrium.

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Polystyrene-supported Selenides and Selenoxide:Versatile Routes to Synthesize Allylic Alcohols

Wei Ming XU, You Chu ZHANG, Xian HUANG

中国化学快报. 2003, 14(08): 797-799.

摘要 ( )

可视化

Several polystyrene-supported selenides and selenoxide have been prepared firstly. These novel reagents were treated with LDA to produce selenium stabilized carbanions, which reacted with aldehydes and alkyl halides, followed by selenoxide syn-elimination and [2,3] sigmatropic rearrangement respectively to give Z-allylic alcohols stereoselectively.

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Regioselective Addition of Silyl Enolates to α,β-Unsaturated Aldehyde and its Acetal Catalyzed by MgI₂ Etherate

Xing Xian ZHANG, Wei Dong Z. LI

中国化学快报. 2003, 14(08): 800-803.

摘要 ( )

可视化

Regioselective addition reactions of silyl enolates to α,β-unsaturated aldehyde and its acetal catalyzed by MgI₂etherate give aldol adducts (1, 2-addition) preferentially over Michael adducts (1, 4-addition). This unique regioselectivity is distinctly different with other Lewis acidic promoters and may be attributed to the high oxyphilicity of IMg⁺.

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Biotransformation of 14-Deacetoxy-13-oxo sinenxan A by Ginkgo Cell Cultures

Jun Gui DAI, Meng ZHANG, Min YE, Wei Hua ZHU, Ji Yu GUO, Xiao Tian LIANG

中国化学快报. 2003, 14(08): 804-806.

摘要 ( )

可视化

14-Deacetoxy-13-oxo sinenxan A (1) was converted to 9α-hydroxy-13-oxo-2α, 5α, 10β-triacetoxy-4(20),11-taxadiene (2) and 10β-hydroxy-13-oxo-2α,5α,9α-triacetoxy-4(20), 11-taxadiene (3) by Ginkgo cell suspension cultures in 45% and 15% yields, respectively.

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A New Poly Brominated Dibenzylphenol from Rhodomela confervoides

Nian Jun XU, Xiao FAN, Yong Chun YANG, Jian Gong SHI

中国化学快报. 2003, 14(08): 807-809.

摘要 ( )

可视化

A new poly brominated dibenzylphenol named as rhodomevoidin was isolated from Rhodomela confervoides. Its structrue was elucidated as 3-bromo-4,5-bis (2,3-dibromo-4,5-dihydroxybenzyl)pyrocatechol by spectroscopic methods including IR, HRFABMS, 1D and 2D NMR techniques.

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Two Benzyl Dihydroflavones from Phellinus igniarius

Shun Yan MO, Wen Yi HE, Yong Chun YANG, Jian Gong SHI

中国化学快报. 2003, 14(08): 810-813.

摘要 ( )

可视化

Two new benzyl dihydroflavones phelligrins A and B were isolated from the fruit body of Phellinus igniarius. Their structrues were identified as 5,7,4'-trihydroxy-6-O-hydroxybenzyl-dihydroflavone and 5,7,4'-trihydroxy-8-O-hydroxybenzyldihydroflavone, respectively, by means of spectral methods.

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Two New Tartrate Derivative Glucosides from Coeloglossum viride (L.) Hartm.var.bracteatum (Willd.) Richter

Sheng Yang HUANG, Jian Gong SHI, Yong Chun YANG, Peng Fei TU

中国化学快报. 2003, 14(08): 814-817.

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可视化

Two new tartrate derivative glucosides, coelovirin C (1) and D (2), were isolated from rhizomes of Coeloglossum viride (L.) Hartm. var. bracteatum (Willd.) Richter (Orchidaceae). Their structures were elucidated as (2R, 3S)-2-β-D-glucopyranosyl-2-isobutyltartrate-1-(4-β-D-glucopyranosyloxybenzyl) ester 1 and (2R, 3S)-2-β-D-glucopyranosyl-2-isobutyltartrate-4-(4-β-D-glucopyranosyloxybenzyl) ester 2 by means of chemical and spectroscopic methods.

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A New Sesquiterpene and a New Norsesquiterpene from Cacalia deltophylla

Ying WANG, Cheng Shan YUAN, Xiao Long WANG, Zhong Jian JIA

中国化学快报. 2003, 14(08): 818-819.

摘要 ( )

可视化

A new sesquiterpene and a new norsesquiterpene were isolated from the whole plant of Cacalia deltophylla (Maxim) Mattf. Their structures were elucidated as deltocacalone (1) and deltonorcacalol (2) by spectroscopic methods including 2D NMR.

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A Bidenate Amide Bonded Stationary Phase for HPLC

Yan Shun MA, Yuan De LONG, Yong Liang DING, Tian Bao HUANG

中国化学快报. 2003, 14(08): 820-823.

摘要 ( )

可视化

A novel bonded stationary phase, bidenate amide bonded stationary phase (BABSP), was prepared by reacting YWG silica gel firstly with 3-aminopropyltrimethoxysilane, then with diacid chloride. Hydrophobicity, selectivity, and especially silanophilic activity of BABSP were evaluated. The stationary phase exhibited good column efficiency and peak shape for separation of some basic solutes.

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Studies on the Renaturation with Simultaneous Purification of Recombinant Human Proinsulin with Unit of Simultaneous Renaturation and Purification of Protein in Semi-preparative Scale

Quan BAI, Yu KONG, Xin Du GENG

中国化学快报. 2003, 14(08): 824-827.

摘要 ( )

可视化

The renaturation and purification of recombinant human proinsulin (rh-proinsulin) expressed in E. Coli with the unit of simultaneous renaturation and purification of protein (USRPP) in semi-preparative scale was studied. The result shows that rh-proinsulin extracted with 8.0 mol/L urea can be renatured and purified simultaneously in 45 minutes with the USRPP (10×50 mm ID). The purity of rh-proinsulin was found to be more than 90% and the mass recovery to be more than 80%. The renaturation effect of rh-proinsulin with the USRPP was tested by enzyme cleavage for obtaining insulin. In addition, the result was further confirmed with RPLC, SDS-PAGE electrophoresis, and MALDI-TOF, respectively.

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Refolding of Denatured/Reduced Lysozyme Using Weak-Cation Exchange Chromatography

Yan WANG, Bo Lin GONG, Xin Du GENG

中国化学快报. 2003, 14(08): 828-831.

摘要 ( )

可视化

Oxidative refolding of the denatured/reduced lysozyme was investigated by using weak-cation exchange chromatography (WCX). The stationary phase of WCX binds to the reduced lysozyme and prevented it from forming intermolecular aggregates. At the same time urea and ammonium sulfate were added to the mobile phase to increase the elution strength for lysozyme. Ammonium sulfate can more stabilize the native protein than a common eluting agent, sodium chloride. Refolding of lysozyme by using this WCX is successfully. It was simply carried out to obtain a completely and correctly refolding of the denatured lysozyme at high concentration of 20.0 mg/mL.

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Recognition of Biotin-functionalized Liposomes

Hai Feng ZHU, Jun Bai LI

中国化学快报. 2003, 14(08): 832-835.

摘要 ( )

可视化

Functionalized liposomes were prepared by mixing the biotin in the lipid vesicle suspensions. The experiments through immersing streptavidin deposited mica into the biotin modified liposome solution testify the specifically biological binding interaction and extend the function of liposomes as a biosensor or drug carrier.

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Effect of Cationic Surfactant on the Inhibition of Ligninase by Hydrogen Peroxide

Zhuan Ni YU, Xi Rong HUANG, Shao Fang SONG, Dan WANG, Xue Mei LU, Yue Zhong LI, Yin Bo QU, Pei Ji GAO

中国化学快报. 2003, 14(08): 836-839.

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可视化

The inhibition of ligninase by hydrogen peroxide in the presence of cationic surfactant CTAB was studied by kinetic spectrophotometric technique. Results showed that addition of CTAB enhanced the inhibition by H₂O₂, but it did not alter the inhibition pattern and the inhibition constant changed little with the concentration of CTAB. Modification of the enzymic protein by the surfactant monomer may be responsible for the above mentioned results.

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Diorgano,Dichloro-tin (Ⅳ) Complexes of 4-X-Benzohydroxamic Acid (X=Cl,OCH₃):Synthesis,Characterization,Antitumor Activity in Vitro and the Crystal Structure of trans-[Me₂Sn(L₂)₂]

Jing Hua ZHAO, Tai Gang LIANG, Qing Shan LI, Armando J. L. Pombeiro

中国化学快报. 2003, 14(08): 840-843.

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可视化

A series of diorganotin (Ⅳ) derivatives of R₂SnL₂ (R=Me, Et, n-Bu, ph or Cl; L=L₁ or L₂) and their corresponding mixed-ligand complexes R₂Sn(L₁)(L₂) have been prepared and the structure of trans-Me₂Sn(L₂)₂ was characterized by FT-IR, ¹H, ¹³C and ¹¹⁹Sn NMR spectroscopies, MS, elemental analysis, melting points and X-ray diffraction. The structure-activity relationships were discussed.

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Porphyrins in Reverse Micelles:the Side-chain Length and the Triplet-state Lifetime

Jun Hua YU, Yu Xiang WENG, Xue Song WANG, Lei ZHANG, Bao Wen ZHANG, Yi CAO

中国化学快报. 2003, 14(08): 844-847.

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可视化

Using bis(2-ethylhexyl) sodium sulfosuccinate (AOT) as surfactant, two amphiphilic porphyrin terminated with imidazole were studied in AOT/iso-octane/water reverse micelles, intending to mimic the relationship between microenvironments in organism and the amphiphilic properties of porphyrins for photodynamic therapy drugs.

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A Large Conformational Change of a Bridged β-Cyclodextrin Dimer in Aqueous Solution

Xiao Qi ZHENG, Yong Hui WANG, Qing Xiang GUO, Li YANG, You Cheng LIU

中国化学快报. 2003, 14(08): 848-851.

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可视化

A novel bridged β-CD dimer in which two β-cyclodextrins were linked by a naphthalene at positions 2 and 7 has been synthesized.¹H and ¹³CNMR measurements showed that a large change in the conformation of the dimer occurred in aqueous solution. The dimer interacted with methyl and ethyl orange to form stable inclusion complexes via "induced fit" mechanism.

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Deposition of Layer-by-layer Inorganic-organic Nano-hybrid Ultrathin Films onto SBA-15

Han Ming DING, Li Ping WANG, Yong Kui SHAN, Ming Yuan HE

中国化学快报. 2003, 14(08): 851-855.

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可视化

Deposition of inorganic-organic nano-hybrid ultrathin films onto mesoporous silicate materials has been proven possible by using layer-by-layer assembly method. In combination with sol-gel method, titania, subsequently dye molecules (or polymer) were successfully fabricated onto the inner wall of SBA-15. Their structures were preliminarily characterized by FTIR and solid-state UV-Vis spectroscopy, thermal analysis, and BET surface area measurements, respectively.

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The Structure and Nonlinear Optical Properties of Octupolar Compound:2,4,6-Tristyryl-s-triazine

Yue Zhi CUI, Qi FANG, Hong LEI, Gang XUE, Wen Tao YU

中国化学快报. 2003, 14(08): 856-859.

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可视化

The crystal of 2,4,6-tristyryl-s-triazine (TSTA) has been prepared and its crystal structure been determined to be in the polar non-centrosymmetric space group Cmc2₁. The molecular structure of TSTA is characterized by the slightly curved planar configuration and the octupolar C_3v molecular symmetry. As expected, TSTA crystal shows a quite novel nonlinear optical (NLO) property with its powder second harmonic generating (SHG) intensity of 1.8 times as that of urea. It also shows excellent transparency (with the peak position of 322 nm in absorption spectrum) and good thermal stability (with the melting point of 225-229℃).

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Two Novel Isomers of HPS₃ System

Hai Tao YU, Ming Xia LI, Yu Juan CHI, Fu Long YUANG, Hong Gang FU, Jia Zhong SUN

中国化学快报. 2003, 14(08): 860-862.

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可视化

Two new isomers of HPS₃ system, HP(S)S₂ and HSSPS, are predicted by means of B3LYP method with 6-311++G(3df,3pd) basis set. The two isomers can isomerize into thermodynamically the most stable species HSPS₂, which have been experimentally identified, with relatively higher reaction barriers. In view of their higher thermodynamical and kinetic stability and the experimental observation for HP(O)O₂ and HOOPO in previous study, we can reasonably believe that the two species can be spectrosymmetrically characterized in future experiments.

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Preparation of MMA-BA-DMAEMA Nanosized Latex

Yu Yang LIU, Mu Jie YANG

中国化学快报. 2003, 14(08): 863-865.

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可视化

The terpolymer latex of methyl methacrylate (MMA)/butyl acrylate (BA)/dimethyl aminoethyl methacrylate (DMAEMA) with diameter of less than 100 nm was prepared by seeding semi-continuous emulsion copolymerization using APS (ammonium persulfate)/TMEDA (N,N,N, N-tetramethylethylenediamine) as the redox initiators and SDS (sodium dodecylsulfate) and OP (P-octylpolyethylene glycol phenylether) as co-emulsifiers. The factors that influenced the process stability of the copolymerization and the particle size of the latex were investigated. The addition of aqueous ammonia as coagulation inhibitor provided better process stability of the copoly-merization. The addition of acetic acid as the acidification agent caused a remarkable reduction of the latex particle size.

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Preparation of Gold Nanoparticles Protected with Polyelectrolyte

Xu Ping SUN, Zhe Ling ZHANG, Bai Lin ZHANG, Xian Dui DONG, Shao Jun DONG, Er Kang WANG

中国化学快报. 2003, 14(08): 866-869.

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可视化

Gold nanoparticles were synthesized through the reduction of tetrachlorauric acid (HAuCl₄) by NaBH₄, with polyethyleneimine(PEI) as stabilizer. The nanoparticles were characterized by UV-vis spectroscopy and atomic force microscopy(AFM).

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An Empiric Linear Formula between the Internal Tetrahedron Symmetric Stretch Frequency and the Al Content in the Framework of KL Molecular Sieves

Nong Yue HE, Chun YANG, Jian Xin TANG, Peng Feng XIAO, Hong CHEN

中国化学快报. 2003, 14(08): 870-873.

摘要 ( )

可视化

KL molecular sieves with different framework compositions were secondarily synthesized by substituting Si for Al with a solution of (NH₄)₂SiF₆. The internal tetrahedron symmetric stretch frequency, at ~770 cm^-1, is linear with the molar fraction of Al (X_Al=Al/(Si+Al)) in the framework of KL samples:X_Al=-7.309×10^-3 (υ₇₇₀-760)+0.3242.

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Synthesis of Compact NaA Zeolite Membrane by Microwave Heating Method

Zhi Lin CHENG, Zi Sheng CHAO, Hui Lin WAN

中国化学快报. 2003, 14(08): 874-876.

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可视化

A continuous and dense NaA zeolite membrane was synthesized by microwave heating method while employing a multi-step seeding LTA zeolite with the average size of 120 nm. The gas H₂/N₂ mixture separating results indicated that the mixture selectivity increased with increasing of synthesis times. In addition, selectivity of the three-step synthesis was higher than the value(3.74) expected from Kundsen diffusion.

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The Intelligent Properties of Micro-reactors for Preparating Nanoparticles

Gang WEI, Hai Yan HUANG, Rong Chun XIONG

中国化学快报. 2003, 14(08): 877-880.

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可视化

TiO₂ nanoparticles were synthesized by using micro-reactors. The shape and size of the nanoparticles produced from the original micro-reactors and the five times recycled micro-reactors mother liquor were investigated on transmission electron microscopy (TEM) by using the original sample, freeze prepared sample, and dyeing treated sample, respectively. UV-VIS spectrometry was used to study the growth process of TiO₂ nanoparticles in main reactors. The results showed that micro-reactors with nanometer magnitude had spherical or oval structures, and could restore to their original structure after they were destroyed. The products prepared in the original micro-reactors were similar to that in the micro-reactors recycled for many times, suggesting that the micro-reactors had memory function.

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2003年, 第14卷, 第08期　刊出日期：2003-08-20

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2003年, 第14卷, 第08期 刊出日期：2003-08-20

2003年, 第14卷, 第08期　刊出日期：2003-08-20