中国化学快报

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Solid-Phase Stereoselective Synthesis of (E)-1,2-Disubstituted Ethenes from Polymer-Sopported α-Selenoaldehydes

Shou Ri SHENG, Lu Ling WU, Xian HUANG

中国化学快报. 2003, 14(10): 991-992.

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Reaction of polymer-supported α-selenoaldehydes with Grignard reagents affordedpolymer-bound β-hydroxyalkyl selenides, which treated with thionyl chloride and triethylamineleading to (E)-1, 2-disubstituted ethenes in good yield.

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Microwave-assisted Solventless Biginelli Reaction Catalyzed by Montmorillonite Clay-SmCl₃·6H₂O System

Yu Xia LI, Wei Liang BAO

中国化学快报. 2003, 14(10): 993-996.

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4-Aryl/alkyl-3, 4-dihydro-2(1H)-pyrimidone esters and 5-acetyl-4-aryl/or alkyl-6-methyl-3, 4-dihydropyrimidin-2(1)-ones were synthesised efficiently using montmorillonite clay-SmCl₃ 6H₂O system promoted by microwave irradiation in solventless condition.

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Study on the Total Synthesis of Et 743 and its Analogues:Synthesis of a Tricyclic Intermediate and its 11-Epimer

Ye Feng TANG, Zhan Zhu LIU, Shi Zhi CHEN

中国化学快报. 2003, 14(10): 997-998.

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The tricyclic compound 1, a key intermediate of the pentacyclic core of Et 743 and its analogues, was synthesized. Its 11-epimer was found as the product of racemization when BOP was used as the coupling agent, but not when BOP-Cl used in the same reaction. The stereochemistry of both isomers was confirmed on basis of the 1H NMR and NOE-difference spectra.

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Design and Synthesis of 3, 4-Dihydropyrrolo[2, 1-c][1,4]oxazin-1-one and its 7-Acyl Derivatives

Yong En GUO, Bin FU, Ying Xiang LIU

中国化学快报. 2003, 14(10): 999-1001.

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Starting from 1H-pyrrole, unreported 3, 4-dihydropyrrolo[2, 1-c][1, 4]oxazin-1-one 4, 7-(4-chlorobenzoyl)-3, 4-dihydropyrrolo[2, 1-c][1, 4]oxazin-l-one 5 and 7-benzoyl-3, 4-dihydro-pyrrolo [2, 1-c][1, 4]oxazin-1-one 9 were designed and synthesized. They may have antipyretic and analgesic activities.

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Synthesis of 2-Arylimidazo[1,2-a]pyrimidines in Ionic Liquids

Dan Qian XU, Bao You LIU, Zhen Yuan XU

中国化学快报. 2003, 14(10): 1002-1004.

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Room temperature ionic liquids were used as a "green" recyclable alternative to conventional solvents in the synthesis of pharmaceutically useful compounds 2-arylimidazo[1, 2-a]pyrimidines through Tschotschibabin reaction of α-bromoacetophenones with 2-aminopyfinidinein good yields.

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A Novel Green Preparation of α,α'-Bis (substituted benzylidene)-cycloalkanones Promoted by FeCl₃·6H₂O in Ionic Liquid

Xin Ying ZHANG, Xue Sen FAN, Hong Ying NIU, Jian Ji WANG

中国化学快报. 2003, 14(10): 1005-1007.

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α, α'-Bis(substituted benzylidene)cycloalkanones were efficiently prepared fromcycloalkanones and benzaldehydes in [bmim][BF₄] by using iron(Ⅲ) chloride hexahydrate as acatalyst. It is shown that [bmim][BF₄] and iron(Ⅲ) chloride hexahydrate can be quantitativelyrecovered and be reused effectively for many times. Compared with the known methods, thisnovel process has the advantage of being an environmentally benign process together with goodyields and mild reaction conditions.

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Asymmetric Dihydroxylation of Allylamine Catalyzed by Wool-OsO₄Complex

Ju Hong MIAO, Ji Huo YANG, Li Yi CHEN, Mei Yu HUANG, Ying Yan JIANG

中国化学快报. 2003, 14(10): 1008-1011.

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A new chiral polymer-metal complex, wool-osmium tetroxide(wool-OsO₄) complex was prepared by a very simple method. This complex was found to be able to catalyze the asymmetric dihydroxylation of allylamine to get (R)-(+)-3-amino-1, 2-propanediol. The experimental results showed that OsO₄ content in the complex, reaction time, allylamine/OsO₄ molar ratio all have great effects on the chemical and optical yields of product. Additionally, wool-OsO₄ complex catalyst could be reused without remarkable change in optical catalytic activity.

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An Efficient Synthesis of Diaryl Ethers by Coupling Aryl Halides with Substituted Phenoxytrimethylsilane in the Presence of TBAF

Jian Kui ZHAO, Yan Guang WANG

中国化学快报. 2003, 14(10): 1012-1014.

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A general synthesis of diaryl ethers via coupling of aryl halides with substituted phenoxytrimethylsilane in the presence of TBAF is described. The protocol is simple and mild, and gives good to excellent yields.

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The Reduction of a Natural Diterpene Containing α, β-Unsaturated Keto Group

Qing ZHAO, Xin HONG, Cheng ZOU, Yue Mao SHEN, Xiao Jiang HAO

中国化学快报. 2003, 14(10): 1015-1017.

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Hedychenone (1), a diterpene containing α, β-unsaturated keto group, was reduced by aluminum-mercury alloy, and a dimerized product (2) was obtained as the major product. The coupling occurred at β position of the keto group.

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Reductive Deoxygenation of Carbonyl to Methylene by LiAlH₄/InBr₃

Nan Yan FU, Xue Mei ZHAO, Yao Feng YUAN, Ji Tao WANG

中国化学快报. 2003, 14(10): 1018-1020.

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The reductive deoxygenation of aldehydes and ketones into the corresponding alkanes is accomplished by LiAlH₄ in the presence of Lewis acid InBr₃. It provides a convenient method to complete the transformation from carbonyl compounds to alkanes.

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Ring-opening Polymerization of ε-Caprolactone Using Lanthanide Tris(4-tert-butylphenolate)s as a Single-component Initiator

Cui Ping YU, Li Fang ZHANG, Zhi Quan SHEN

中国化学快报. 2003, 14(10): 1021-1023.

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The ring-opening polymerization of ε-caprolactone (CL) initiated by novel single lanthanide tris(4-tert-butylphenolate)s [Ln(OTBP)₃] is reported. Single-component La(OTBP)₃ can effectively prepare polycaprolactone (PCL) with over 90% yield and viscosity average molecular weight about 60×10³ under quite mild conditions:molar ratio of CL to initiator is 1000, 60℃, 2 h in toluene. Mechanism study indicates that the monomer inserts into the growing chain via the break of acyl-oxygen bond of CL.

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A Novel Fluorescent Probe for Lead Ions

Ming SUN, Di Hua SHANG GUAN, Hui Min MA, Li Hua NIE, Xiao Hua LIShao Xiang XIONG

中国化学快报. 2003, 14(10): 1024-1026.

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A new fluorescent probe for lead ions, p-nitrophenyl 3H-phenoxazin-3-one-7-yl phosphoric acid (NPPA), has been synthesized by linking resorufin (serving as a fluorophore and electron acceptor) to p-nitrophenol (serving as a fluorescence quencher and electron donor) through phosphodiester bonds. When NPPA was irradiated with light, intramolecular fluorescence self-quenching took place due to the PET (photoinduced electron transfer) from the donor to the acceptor. However, upon addition of Pb^Ⅱ, the phosphate ester bonds in the probe were cleaved and the fiuorophore was released, accompanying the retrievement of fluorescence.

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A Novel Pregnane Glycoside from Biondia chinensis

Xing Gen TAN, Shu Lin PENG, Xun LIAO, Jian LIANG, Li Sheng DING

中国化学快报. 2003, 14(10): 1027-1028.

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A novel pregnane glycoside, biondianoside E, was isolated from the roots of Biondia chinensis. By the spectroscopic and chemical methods, this structure was elucidated as 3β, 5β, 14β, 20S, 21-pentahydroxypregnane 3-O-β-D-glucopyranosyl-(1→4)-β-D-cymaropyranoside.

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Two New Monoterpene Diglycosides from Winchia calophylla A. DC

Wei Ming ZHU, Bin Gui WANG, Wen Yi KANG, Xin HONG, Jun ZHOU, Xiao Jiang HAO

中国化学快报. 2003, 14(10): 1029-1032.

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Two new monoterpene diglycosides, wincaloside A (1) and wincaloside B (2), along with loganin (3) were isolated from the stem barks of Winchia calophylla A. DC. The structures of 1 and 2 were established by spectroscopic and chemical methods.

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One New A-type Proanthocyanidin Trimer from Lindera aggregata (Sims) Kosterm

Chao Feng ZHANG, Qi Shi SUN, Zheng Tao WANG, Masao HATTORI

中国化学快报. 2003, 14(10): 1033-1036.

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One new A-type proanthocyanidin trimer, lindetarmin trimer, was isolated from the stems of Lindera aggregata (Sims) Kosterm.. Its structure was elucidated by spectral and chemical methods.

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Two New Sterols from Bolbostemma paniculatum

Wen Yong LIU, Wei Dong ZHANG, Hai Sheng CHEN, Zheng Ring GU, Ting Zhao LI, Wan Sheng CHEN

中国化学快报. 2003, 14(10): 1037-1040.

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Two new sterols were isolated from bulbs of Bolbostemma paniculatum (Maxim.) Franquet. Their structures were elucidated as stigmasta-7, 22, 25-triene-3-O-nonadecanoic acid ester (1) and stigmasta-7, 22, 25-triene-3-O-β-D-(6'-palmitoyl) glucopyranoside (2) by chemicaland spectroscopic methods.

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Oleanane-triterpene Saponins from Clinopodium urticifolium

Li Ming GAO, Xiao Mei WEI, Dong Liang CHENG

中国化学快报. 2003, 14(10): 1041-1044.

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Four new oleanane triterpene saponins were isolated and purified from the whole plant of Clinopodium urticifolium. They were 3β, 16β, 23, 28-tetrahydroxyoleana-9 (11), 12(13)-diene-3-yl-[β-D-glucopyranosyl-(1→2)]-[β-D-glucopyranosyl-(1→3)]-β-D-fucopyranoside 1;3β, 16β, 21β, 23, 28-pentahydroxyoleana-9(11), 12(13)-diene-3-yl-[β-D-glucopyranosyl-(1→2)]-[β-D-glucopyranosyl-(1→3)]-β-D-fucopyranoside 2;3β, 16β, 23, 28-tetrahydroxyoleana-9(11), 12(13)-diene-3-yl-[β-D-glucopyranosyl-(1→6)-β-D-glucopyranosyl-(1→3)]-[β-D-glucopyranosyl-(1→2)]-β-D-fucopyranoside 3;3β, 16β, 23, 28-tetrahydroxyoleana-9(11), 12(13)-diene-3-yl-[β-D-gluco-pyranosyl-(1→4)-β-D-glucopyranosyl-(1→6)-β-D-glucopyranosyl-(1→3)]-[β-D-glucopyranosyl-(1→2)]-β-D-fucopyranoside 4. Their structures were elucidated on the basis of interpretation of NMR and MS data and from chemical evidence.

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A New Brominated Phenylpropylaldehyde and its Dimethyl Acetal from Red Alga Rhodomela confervoides

Xiao FAN, Man Jun XU, Jian Gong SHI

中国化学快报. 2003, 14(10): 1045-1047.

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A new brominated phenylpropylaldehyde and its dimethyl acetal together with a new natural brominated phenol were isolated from Rhodomela confervoides. Their structrues were elucidated as 2-methyl-3-(2,3-di bromo-4,5-dihydroxyphenyl)propylaldehyde, 2-methyl-3-(2,3-di-bromo-4,5-dihydroxyphenyl) propylaldehyde dimethyl acetal and 3-bromo-4,5-dihydroxybenzoic acid methyl ester by spectroscopic techniques including IR, HRFABMS, 1D and 2DNMR experiments.

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A New Stilbene Tetramer from Caragana rosea

Guo Xun YANG, Chang Qi HU

中国化学快报. 2003, 14(10): 1048-1050.

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Cararosinol A, a new stilbene tetramer, was isolated from Caragana rosea. Itsstructure has been established on the basis of spectroscopic evidence.

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Flow-injection Chemiluminescence Determination of Trace Calf Thymus DNA

Min ZHOU, Yong Jun MA, Xiao Yong JIN, Xiu Lan TENG, Zi Yu ZHANG, Hui CHEN

中国化学快报. 2003, 14(10): 1051-1053.

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A flow injection procedure for the determination of calf thymus DNA (CT DNA) over the range 2.1×10^-6~2.1×10^-1 μg mL^-1 is described, based on measurement of the enhanced chemiluminescence emission of rhodamine B-Ce(Ⅳ) system, activated by imidazole-HCl buffer solution. This method is highly sensitive, with the linearity range broadened to five orders of magnitude. It has been applied to determine CT DNA in synthetic sample with satisfactory results.

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Interaction of Hypocrellin B or Mono-cysteine Substituted Hypocrellin B with CT-DNA by Spectral Methods

Jia Hong ZHOU, Sheng Qin XIA, Xue Song WANG, Bao Wen ZHANG, Yi CAO

中国化学快报. 2003, 14(10): 1054-1057.

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The interaction of the anticancer drag hypocrellin B (HB) or the mono-cysteine substituted hypocrellin B (MCHB) and calf thymus deoxyribonucleic acid (CT-DNA) has been investigated using spectral methods. The results of UV-visible spectra show that the HB and MCHB could intercalate into the base-stacking domain of the CT-DNA double helix. The studies of fluorescence spectra and circular dichroism(CD) spectra also support the interacalation mechanism.

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Effect of Low Energy Electron Exposure on Ion Scattering Spectroscopy

Li Mei QIU, Fen LIU, Liang Zhong ZHAO

中国化学快报. 2003, 14(10): 1058-1061.

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The effect of low energy electron (LEE) exposure on ISS, including on the sputter peak and scatter peak as well as on ion neutralization, has been investigated for different samples.Some new results are discussed.

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Nonlinear Behavior and Domain Feature at Oil/Water Interface

Jin Zhang GAO, Kan Jun SUN, Wu YANG

中国化学快报. 2003, 14(10): 1062-1065.

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Studies on nonlinear behavior at oil/water interface membrane were performed. This system showed rhythmic oscillations and chaos of electrical potential in a given concentration domain. The nonlinear behavior response at the liquid membrane apparently resembled that of biological chemoreceptive membrane. The possibility of developing a new type of chemical sensor with the ability to simulate substance equilibrium in living organisms was suggested in the paper.

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Selective Oxidation of Methane to Methanol Using Molecular Oxygen on MoO_x/(LaCoO₃+Co₃O₄) Catalysts

Xin ZHANG, De Hua HE, Qi Jiang ZHANG, Bo Qing XU, Qi Ming ZHU

中国化学快报. 2003, 14(10): 1066-1069.

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Comparatively high CH₃OH selectivity (60.0%) and yield (6.7%) were obtained on MoO_x/(LaCoO₃+Co₃O₄) catalysts in selective oxidation of methane to methanol using molecular oxygen as oxidant. The interaction between MoO_x and La-Co-oxide modified the molecular structure of molybdenum oxide and the ratio of O^-/O^2- on the catalyst surface, which controlled the catalytic performance of MoO_x/(LaCoO₃+Co₃O₄) catalysts.

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Oxidation of n-Butanol and 2-Pentanol with Molecular Oxygen in Supercritical CO₂

Yan Hong CHANG, Tao JIANG, Liang GAO, Quo Ying ZHAO, Hai Xiang GAO, Zhong Hao LI, Jun Chun LI, Zhi Min Liu, Bu Xing HAN

中国化学快报. 2003, 14(10): 1070-1072.

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Oxidation of n-butanol and 2-pentanol using molecular oxygen in supercritical (SC) CO₂ with and without co-solvent is investigated. The results showed that the reaction selectivity is high when the reaction is carried out in SC CO₂. It has been observed that co-solvent affects conversion and selectivity of the reaction considerably.

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Effects of Bases on the Stabilities of Nucleoside C4'Radicals

Bo Lin LIN, Yao FU, Lei LIU, Qing Xiang GUO

中国化学快报. 2003, 14(10): 1073-1076.

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C4'-H bond dissociation enthalpies of nucleosides were predicted using theoretical methods to a precision of 1-2 Kcal/mol. It was found that the stability of the C4'nucleoside radical is slightly dependent on the base. The orders of stability are dA < dG < dT < dC for deoxynucleosides and U < G < A≈C for nucleosides.

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Molecular Exchanging Energy of Anionic/Cationic Surfactants System on the Surface of Solution

Zheng Wu WANG, Dong Yang HUANG, Xi Zhang YI

中国化学快报. 2003, 14(10): 1077-1080.

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In order to study synergism of the mixed suffactants system with molecular exchanging energy (ε), the Lennard-Jones formula has been firstly introduced to evaluate the ε of the mixed system, CH₃(CH₂)_nOSO₃^-/CH₃(CH₂)_nN⁺(CH₃)₃, directly from their molecular structure. The comparison of the calculated and the observed results showed that this method is practical.

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Study on the Reaction Mechanism for Carbon Dioxide Reforming of Methane over supported Nickel Catalyst

Ling QIAN, Zi Feng YAN

中国化学快报. 2003, 14(10): 1081-1084.

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The adsorption and dissociation of methane and carbon dioxide for reforming on nickel catalyst were extensively investigated by TPSR and TPD experiments. It showed that the decomposition of methane results in the formation of at least three kinds of surface carbon species on supported nickel catalyst, while CO₂ adsorbed on the catalyst weakly and only existed in one kind of adsorption state. Then the mechanism of interaction between the species dissociated from CH₄ and CO₂ during reforming was proposed.

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A Kinetic Evidence for the Nitroxyl Radicals Recycling Mechanism in the Photostabilizing Process of HALS

Xiao Xuan LIU, Xing Hong ZHANG, Guang Guo WU, Jian Wen YANG, Zhao Hua ZENG, Yong Lie CHEN

中国化学快报. 2003, 14(10): 1085-1088.

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The photoinduced bulk polymerization of a reactive-hindered amine light stabilizers(r-HALS), 4-acryloyl-2, 2, 6, 6-tetramethylpiperidinyl (ATMP), was performed at 80℃ by using a DPC technique. An unique periodic exponential attenuation-type oscillating curve was found when the polymerization was carried out in air, but this phenomenon was not found in nitrogen.It is supposed that this unique kinetic performance may be attributed to nitroxyl radicals that are produced in situ from the oxidation of ATMP. ATMP polymer with narrow polydispersity (d=1.03) can be obtained by photoinduced solution polymerization of ATMP. The signal detected in ESR may be assigned to the nitroxyl radicals in the matrix of ATMP polymer. Since this kind of recycling of nitroxyl radicals is well documented for the photostabilizing mechanism of HALS, the present results may serve as a kinetic evidence for this mechanism.

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Synthesis, Structure and Conductivity of (PyH)[Ni(dmit)₂]₂

Wen XU, Qi FANG, Gang XUE, Wen Tao YU, Hong Yu CHEN, Guo Qun LIU, Wei XU, Cui Ying XU, De Qing ZHANG, Dao Ben ZHU

中国化学快报. 2003, 14(10): 1089-1092.

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A new molecular conductor (PyH)[Ni(dmit)₂]₂(dmit=4, 5-dimercapto-1, 3-dithiole-2-thione) has been prepared and its crystal structure has been determined. Crystallographic parameters for (PyH)[Ni(dmit)₂]₂:C₁₇H₆NNi₂S₂₀;triclinic system;P-1 space group;a=5.9227 (4), b=8.2279 (6), c=16.7535 (9)Å, α=90.233 (5)°, β=92.107 (6)°, γ=104.654 (6) °;V=789.25 (9) Å³;Z=1;D_c=2.068 g/cm³;F(000)=491. The conductivity at one direction on (001) plane at room temperature was measured to be 0.13 Ω^-1·cm^-1. The resistivity-temperature curve in the temperature range of 90~290 K shows that this compound behaves as a semiconductor.

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Dye-sensitized TiO₂Solid Solar Cell Using Poly (4-vinylphenyloxy-methyltriphenylamine) as Hole Transport Material

Ke Jian JIANG, Ya Li SUN, Ke Feng SHAO, Jin Fang WANG, Lian Ming YANG

中国化学快报. 2003, 14(10): 1093-1096.

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A dye-sensitized TiO₂ solid solar cell, which contains poly(4-vinylphenyloxy-methyltriphenylamine) in hole transport layer (HTL) doped with LiSCN and methyl-hexyl-imidazolium iodide (MHIml), was prepared. The solar cell shows that the conversion efficiencyis 0.59%, J_sc is 3.03mA/cm², and V_oc is 0.53V at 1 sun light intensity.

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Study on Intercalative Nanohybrid of Cordycepin in Layered Double Hydroxide

Jian Ya LING, Jing YANG, Qin Zheng YANG, Jun Feng PENG, Han Xing ZHANG, Chang Kai ZHANG

中国化学快报. 2003, 14(10): 1097-1100.

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A novel negatively charged biomolecule-cordycepin has been intercalated within the gallery spaces of [Mg-Al-NO₃]. Results of TEM, PXRD and FT-IR spectroscopy confirmed that cordycepin could be intercalated into [Mg-Al-NO₃] interlayers as the charge-compensating species.Initial studies suggest that the new bioinorganic nanocomposite may be used as a novel inorganic reservoir or carrier of pharmaceutically active compounds.

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2003年, 第14卷, 第10期　刊出日期：2003-10-20

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2003年, 第14卷, 第10期 刊出日期：2003-10-20

2003年, 第14卷, 第10期　刊出日期：2003-10-20