2002 Volume 13 Issue 6

4-(Benzylamino)formoyldiphenylammonium Triflate (BDPAT):An Efficient, Recoverable Biphasic Catalyst For Esterification of Carboxylic Acids with Equimolar Amounts of Alcohols
Ming LEI , Cheng MA , Yan Guang WANG
2002, 13(6): 487-488
[Abstract](567) [FullText HTML] [PDF 22KB](1)
Abstract:
Esterification of carboxylic acid with equimolar amounts alcohol can be efficiently catalyzed by biphasic 4-(benzylamino)formoyldiphenylammonium triflate (BDPAT, 3) in good yield. The catalyst can be easily recovered without loss of activity.
Promoter Effects of Rare Earth Ions on Electrocatalytic Oxidation of Methanol
Jing Hua LIU , Wei XING , Hui YANG , Tian Hong LU
2002, 13(6): 489-490
[Abstract](547) [FullText HTML] [PDF 16KB](2)
Abstract:
The promoter effects of rare earth ions on the electrocatalytic oxidation of methanol at the Pt electrode were studied using the cyclic voltammetry and stable polarization techniques. It was found for the first time that Eu Ho Dy ions could accelerate the electrocatalytic oxidation of methanol at the Pt electrode, while Lu Pr Yb Sm ions showed inhibitor effects.
Oxidation of Cyclohexene Catalyzed by PAMAM-SA-M Dendrimers
Zi Qiang LEI , Zhi Wang YANG , Qiao Rong HAN , Zhen GUO , Heng Chang MA , Yong Fu CAI , Yun Pu WANG
2002, 13(6): 491-494
[Abstract](540) [FullText HTML] [PDF 31KB](0)
Abstract:
Oxidation of cyclohexene under 1 atmospheric pressure of molecular oxygen at 70℃ in the absence of solvent catalyzed by PAMAM-SA-M (Where PAMAM=polyamidoamine; SA=salicyaldehyde; M=metal ions Fe3+, Co2+, Ni2+, Mn2+, Cu2+, Zn2+, respectively) dendrimers,afforded 2-cyclohexen-1-ol 1, 2-cyclohexen-1-one 2, 7-oxabicyclo [4,1,0] heptane 3 and 7-oxabicyl [4,1,0] heptan-2-one 4 as the major products. The factors that affect this reaction are also discussed.
Ferric Chloride Catalyzed Isomerization and Cyclization of Geraniol,Linalool and Nerol
Wei YU , Miao WEN , Li YANG , Zhong Li LIU
2002, 13(6): 495-496
[Abstract](1615) [FullText HTML] [PDF 18KB](28)
Abstract:
Ferric chloride catalyzes the isomerization and cyclization of geraniol, linalool and nerol in acetonitrile giving α-terpineol in good to high yields.
Hydroformylation of Oleyl Alcohol Catalyzed by Rh-OPGPP Complex
Fan Zhi KONG , Yan Hua WANG , Zi Lin JIN
2002, 13(6): 497-498
[Abstract](476) [FullText HTML] [PDF 16KB](1)
Abstract:
Polyether-tailored phosphite modified rhodium complex formed in situ was highly active in the hydroformylation of oleyl alcohol in nonaqueous phosphite/heptane system where the phosphite acted both as the ligand and the second phase. This catalyst was easily separated by simple decantation and can be used for five times with only a slight decrease in activity.
Efficient Debromination of Vicinal α, β-Dibromo Carboxylic Acid Derivatives with the Sm/HOAc System
Xiao Xia WANG , Yong Min ZHANG
2002, 13(6): 499-500
[Abstract](488) [FullText HTML] [PDF 19KB](0)
Abstract:
The , vicinal dibromo carboxylic acid and its derivatives were debrominated with Sm/HOAc system to afford the corresponding cinnamic acid and its derivatives in good yields under mild conditions.
A Highly Regioselective Deacetylation of Taxanes
Meng ZHANG , Da Li YIN , Ji Yu GUO , Xiao Tian LIANG
2002, 13(6): 501-504
[Abstract](467) [FullText HTML] [PDF 33KB](0)
Abstract:
A highly regioselective O-deacetylation of taxanes at C-5 position was accomplished by treatment with t-BuOK and a possible mechanism was proposed.
A Practical Synthesis of (S)-(+)-2-(6'-methoxyl-2-naphthyl) propionic Acid
Hong Zhu MA , Bo WANG , Qi Zhen SHI
2002, 13(6): 505-508
[Abstract](484) [FullText HTML] [PDF 32KB](0)
Abstract:
A simplified procedure for enantioselective synthesis of (S)-(+)-2-(6'-methoxyl-2-naphthyl) propionic acid ((S)-(+)-naproxen), starting from (6-methoxy-α-naphthyl)-1-propanone,with D-mannitol as auxiliary catalyzed by SmCl3 in one-pot is described. The yield is 87.5%(ee value 99%).
Synthesis of Multidentate Squaraines
Ying LI , Ming Gui XIE
2002, 13(6): 509-512
[Abstract](487) [FullText HTML] [PDF 99KB](0)
Abstract:
To search for more better sensitizer of organic solar cell, a series of multidentate squaraines (Sq1~6) were synthesized, the structures were determined by elemental analysis, IR,UV-vis, 1H NMR and MS spectroscopies. The squaraines have good solubility in polar solvents such as EtOH, CH3COCH3, CHCl3,etc. as well as strong absorption band over 600~700 nm spectral range.
Synthesis of Tetra-Schiff Base Macrocyclic Compound Containing Benzo-12-crown-4
Bin SUN , Jun Ru CHEN , Hua CHEN , Yao Zhong LI , Xian Jun LI
2002, 13(6): 513-514
[Abstract](511) [FullText HTML] [PDF 62KB](4)
Abstract:
Tetra-Schiff base macrocyclic compound containing benzo-12-crown-4 was synthesized via condensation of 2, 6-diformyl-4-methyl-phenol with 4', 5'-diaminobenzo-12–-C-4 promoted by proton. The compound was characterized by MS, IR 1HNMR spectroscopy and elemental analysis.
New Synthesis of (±)Shikalkin
Hai YANG , Qian LI , Jian Xiong BAO , Wei LU , Haji Aker AISA , Jun Chao CAI
2002, 13(6): 515-518
[Abstract](471) [FullText HTML] [PDF 48KB](1)
Abstract:
The new synthetic route of (±)shikalkin 1 was developed. 3-(1-Hydroxy-4-methyl-3-pentenyl)-5, 8-dimethoxy-1-naphthol 8 was obtained from compound 3 in 10 steps. Then (±)shikalkin 1 was synthesized from 8 in one step with reagents AgO/HNO3 in 1, 4-dioxane.
Enantioselective Total Synthesis of Four Styrylpyrone Derivatives
Xiao Shui PENG , An Pai LI , Tong Xing WU , Xin Fu PAN
2002, 13(6): 519-520
[Abstract](496) [FullText HTML] [PDF 23KB](5)
Abstract:
The first enantioselective total synthesis of 5-acetoxygoniothalamin 1 and 5-acetoxyisogoniothalamin oxide 2 was achieved through the Sharpless kinetic resolution of racemic secondary 2-furylmethanol 5 and the Mitsunobu reaction. At the same time we developed a short synthetic route for 6R-(+)-goniothalamin 3 and (6R, 7R, 8R)-(+)-goniothalamin oxide 4. And according to this route the configuration of 5-acetoxygoniothalamin 1 was confirmed as (5S, 6S).
Studies on the Synthesis of a Natural Product-Piceatannol and its Analogs
Zhi Song PIAO , Lin WANG , Ya Bin FENG , Zhi Zhong ZHAO
2002, 13(6): 521-524
[Abstract](608) [FullText HTML] [PDF 35KB](2)
Abstract:
Piceatannol, (E)-3, 3', 4, 5'-tetrahydroxy stilbene, a natural polyhydroxy stilbene,possesses many biological activities, its synthesis has been reported. We designed another route of its synthesis, which can be controlled more easily. The synthetic product was characterized by elemental analysis, IR, MS and 1H-NMR. Its analogs were synthesized by the similar method.
Synthesis and Conformational Properties of Bis(calix[4]arene)
Qi Yu ZHENG , Chuan Feng CHEN , Zhi Tang HUANG
2002, 13(6): 525-527
[Abstract](506) [FullText HTML] [PDF 74KB](0)
Abstract:
The bis(calix[4]arene) 3 was synthesized in moderate yield by the reaction of p-tert-butylcalix[4]arene (1) with 1,4-bis(chloromethyl)benzene (2). The conformation of all alkylated product 4 was investigated by the variable-temperature 1H-NMR.
Study on the Synthesis of Metabolite of Clausenamide (CM1)
Xing Zhou LI , Ke Mei WU , Dao Fei HUANG , Liang HUANG
2002, 13(6): 528-530
[Abstract](491) [FullText HTML] [PDF 63KB](1)
Abstract:
(+)CM1, (-)CM1 as well as (±)CM1-the metabolites of clausenamide were synthesized from β-phenyl-(N-p-methoxylbenzyl)-ethanol amine through 8 and 6 steps respectively.
1,4-Pyrone Effects on O-H Bond Dissociation Energies of Catechols in Flavonoids: A Density Functional Theory Study
Hong Yu ZHANG , You Min SUN , De Zhan CHEN
2002, 13(6): 531-534
[Abstract](482) [FullText HTML] [PDF 32KB](1)
Abstract:
Through B3LYP/6-31G** calculations, the 1, 4-pyrone effects on O-H bond dissociation energies (BDEs) of catechols in rings A or B of flavonoids were investigated. For the catechol in ring A, although 1, 4-pyrone enlarged the conjugation system, its electron-withdrawing property increased the O-H BDE~3×4.184 kJ/mol compared with that of catechol. However, for the catechol in ring B, 1, 4-pyrone was poorly conjugated with the moiety,and therefore, had little effect on the O-H BDE.
A New Bibenzyl Derivative from Dendrobium moniliforme
Zhi Ming BI , Li YANG , Zheng Tao WANG , Luo Shan XU , Guo Jun XU
2002, 13(6): 535-536
[Abstract](494) [FullText HTML] [PDF 21KB](1)
Abstract:
A new bibenzyl derivative, 3,4-dihydroxy-4',5-dimethoxy bibenzyl, was isolated from a orchid Dendrobium moniliforme. The structure elucidation and 1H,13C NMR assignments were achieved by spectroscopic method.
A Flavonol Glycoside from Smilax glabra
Ting CHEN , Jian Xin LI , Yu CAI , Qiang XU
2002, 13(6): 537-538
[Abstract](507) [FullText HTML] [PDF 23KB](2)
Abstract:
A new flavonol glycoside, named neosmitilbin was isolated form the rhizome of Smilax glabra. Its structure and absolute configuration were elucidated on the basis of spectroscopic studies.
Two New Xanthone Glycosides from Securidaca inappendiculata
Xue Dong YANG , Li Zhen XU , Shi Lin YANG
2002, 13(6): 539-542
[Abstract](474) [FullText HTML] [PDF 28KB](0)
Abstract:
Two new xanthone glycosides, securixanside B and C, were isolated from the stems of Securidaca inappendiculata. Their structures were determined as 3-O-β-D-glucopyranosyl-1,7-dihydroxy-2-methoxyxanthone and 6-O-β-D-glucopyranosyl-1-hydroxy-4,7-dimethoxyxanthone by spectroscopic methods.
Two New C-21 Steroidal Glycosides from Cynanchum aurichulatum
Yue Qi WANG , Xian Zhong YAN , Shu Sheng GONG , Wen Huan FU
2002, 13(6): 543-546
[Abstract](509) [FullText HTML] [PDF 28KB](1)
Abstract:
Two new C-21 steroidal glycosides, cynanauriculoside I and cynanauriculoside Ⅱ, were isolated from the roots of Cynanchum aurichulatum. Their structures were established using spectroscopic methods including one and two-dimensional NMR.
Two New Cardenolide Glycosides from Biondia hemsleyana
Xing Gen TAN , Xiao Rong ZHANG , Ming Kui WANG , Shu Lin PENG , Li Sheng DING
2002, 13(6): 547-548
[Abstract](508) [FullText HTML] [PDF 23KB](4)
Abstract:
Two new cardenolide glycosides, biondianosides A and B, were isolated from the roots of endemic plant of Biondia hemsleyana (Warb.) Tsiang. Their structures were elucidated as periplogenin-3-O-β-D-glucopyranosyl-(1→6)-β-D-glucopyranosyl-(1→4)-β-D-cymaropyranosid e (1) and 17 H-periplogenin-3-O-β-D-cymaropyranoside (2) by the spectroscopic and chemical methods.
Gnetuhainin S, a New Resveratrol Dimer from Gnetum hainanense
Shan ZHOU , Ying Hong WANG , Mao LIN
2002, 13(6): 549-550
[Abstract](508) [FullText HTML] [PDF 21KB](3)
Abstract:
Gnetuhainin S, a new resveratrol dimer, was isolated from the lianas of Gnetum hainanense C. Y. Cheng. Its structure and relative configuration were established on the basis of spectroscopic evidence.
Two New Isobutyltartrate Monoesters from Coeloglossum viride (L.)Hartm. var. bracteatum (Willd.) Richter
Sheng Yang HUANG , Jian Gong SHI , Yong Chun YANG , Shi Lin HU
2002, 13(6): 551-554
[Abstract](509) [FullText HTML] [PDF 32KB](1)
Abstract:
Two new isobutyltartrate monoesters, coelovirin A (1) and B (2), were isolated from the rhizomes of Coeloglossum viride (L.) Hartm. var. bracteatum (Willd.) Richter (Orchidaceae).Their structures were elucidated as (2R, 3S)-2-isobutyltartrate-1-(4-β-D-glucopyranosyloxybenzyl)ester 1 and (2R, 3S)-2-isobutyltartrate-4-(4-β-D-glucopyranosyloxybenzyl) ester 2 on the basis ofphysical constants and spectroscopic methods including 2D NMR techniques.
A New Acyclic Sesquiterpene Oligoglycoside from Pericarps of Sapindus mukurossi
Jie Ru SUN , Kong Chang CHENG , Tie Yin PAN , Xin Mei SI
2002, 13(6): 555-556
[Abstract](478) [FullText HTML] [PDF 21KB](2)
Abstract:
A new acyclic sesquiterpene oligoglycoside, named mukurozioside A, was isolated from pericarps of Sapindus mukurossi. On the basis of chemical and spectral evidence, the structure of mukurozioside A has been established as: 11(S)-2, 6(E, E)-dodecadiene-3, 7, 11-trimethyl-1,12-diol-1,12-bis-O--L-rhamnopyranosyl-(1→2)-[-L-rhamnopyranosyl-(1→3)]-6-O-acetyl--DGlucopyranoside (1).
Analysis of Phthalate Esters in Air, Soil and Plants in Plastic Film Greenhouse
Xi Kui WANG , Wei Lin GUO , Ping Rui MENG , Jia An GAN
2002, 13(6): 557-560
[Abstract](519) [FullText HTML] [PDF 29KB](4)
Abstract:
The phthalate esters such as DMP, DEP, DBP and DEHP in air, soil and plant samples in plastic film greenhouse were clean up with fine silica gel column and determined with HPLC. It was found that the concentrations of PEs in air and soil samples in plastic film greenhouse are much higher than those of contrast samples. But concentrations of PEs in plants in plastic film greenhouse are not remarkably affected by the pollution of air and soil.
A Novel Substrate Used for Simultaneous SERS and RAIR
Jian Ming ZHANG , De Yan SHEN
2002, 13(6): 561-562
[Abstract](483) [FullText HTML] [PDF 31KB](0)
Abstract:
A novel substrate, whose silver particles were deposited on both sides of a slide, was made by silver mirror reaction. Its two sides had different thinness and reflectivity and they were suited for the test of surface enhanced Raman spectroscopy (SERS) and reflection absorption infrared spectroscopy (RAIR) technique respectively.
Near-infrared SERS Study of the Adsorption of a-PMMA Dip-coated onto Silver Mirror Substrate
Jian Ming ZHANG , De Yan SHEN
2002, 13(6): 563-566
[Abstract](499) [FullText HTML] [PDF 41KB](0)
Abstract:
The interface between a-PMMA thin film and silver mirror substrate was investigated using surface-enhanced Raman scattering (SERS). It is found that the molecular chain axis of a-PMMA tends to parallel the substrate in the interface. When the sample is annealed at different temperatures, some interesting changes appear in the SERS spectra. The spectra differences and their transition are due to the surface geometry change of the ester group.
Transient Spectroscopic Properties of [60]Fullerene-Containing Cyclic Sulphoxide
He Ping ZENG , Zhi ZENG , Ding Qiao YANG
2002, 13(6): 567-570
[Abstract](608) [FullText HTML] [PDF 46KB](0)
Abstract:
The properties of the triplet excited state of [60]fullerene-containing cyclic sulphoxide have been investigated by time-resolved absorption spectroscopy. Transient absorption bands of [60]fullerene-containing cyclic sulphoxide showed two decay-components, which were attributed to triplet excited states of different spin multiplicity. The properties of photoexcited states of [60]fullerene-containing cyclic sulphoxide are also reported.
A Spectrometric Setup for Synchronous Total Internal Reflection Fluorescence Measurement at the Solid/Liquid Interface
Yao Qun LI , Jia Ju XU , Run Tang WANG , Li Jun YU , Zhao LI
2002, 13(6): 571-572
[Abstract](505) [FullText HTML] [PDF 40KB](0)
Abstract:
A spectrometric setup to perform total internal reflection fluorescence (TIRF) and synchronous TIRF measurements at solid/liquid interfaces is presented. The combination of TIRF and synchronous fluorescence was proposed to analyze simultaneously different components at interfaces. The TIRF excitation, emission and synchronous spectra of a water-soluble porphyrin were obtained from water/glass interface using this setup without the existence of a surfactant.
Effect of Cationic Surfactant on the Gelation of HPAM by Cr(Ⅲ)
Hong Dong DUAN , Wan Guo HOU , De Jun SUN , Bo Geng LI
2002, 13(6): 573-574
[Abstract](481) [FullText HTML] [PDF 21KB](1)
Abstract:
The effect of cationic surfactant cetyltrimethylammonium bromide (CTAB) on the gelation of partially hydrolyzed polyacrylamide (HPAM) by Cr (Ⅲ) was investigated by using rheological measurements. The results indicated that the CTAB concentration has a pronounced effect on the viscoelastic properties of the gelling system.
Kinetics of Photocatalytic Degradation of Formic Acid over Silica Composite Films Based on Polyoxometalates
Dan Feng LI , Yi Hang GUO , Chang Wen HU , Li MAO , En Bo WANG
2002, 13(6): 575-578
[Abstract](511) [FullText HTML] [PDF 43KB](3)
Abstract:
The composite films, XW11O39n-/SiO2, (X refers to Si, Ge or P, respectively) were prepared by tetraethoxysilane (TEOS) hydrolysis sol-gel method via spin-coating technique.Formation of the composite films is due to strong chemical reaction of organic silanol group with the surface oxygen atoms of XW11O39n-, resulted in the saturation of the surface of the lacunary polyoxometalates (POMs). Therefore, the coordination structural model of the films was proposed. As for the films, retention of the primary Keggin structure was confirmed by UV-vis,FT-IR spectra and MAS NMR. The surface morphology of the films was characterized by SEM,indicating that the film surface is relatively uniform, and the layer thickness is in the range of 250~350 nm. Aqueous formic acid (FA) (0-20 mmol/L) was degraded into CO2 and H2O byirradiating the films in the near-UV area. The results show that all the films have photocatalytic activities and the degradation reaction follows Langmuir-Hinshelwood first order kinetics.
Heterogeneous Catalytic Ozonization of Sulfosalicylic Acid
Shao Ping TONG , Wen Hua LENG , Jiang Qing ZHANG , Chu Nan CAO
2002, 13(6): 579-582
[Abstract](509) [FullText HTML] [PDF 30KB](0)
Abstract:
This paper describes the potential of heterogeneous catalytic ozonization of sulfo-salicylic acid (SSal). It was found that catalytic ozonization in the presence of Mn-Zr-O (a modified manganese dioxide supported on silica gel) had significantly enhanced the removal rate (72%) of total organic carbon (TOC) compared with that of ozonization alone (19%). The efficient removal rate of TOC was probably due to increasing the adsorption ability of catalyst and accelerating decomposition of ozone to produce more powerful oxidants than ozone.
Synthesis and Structure of a New Dinuclear Uranyl Complex
Shang Ying LIU , Yong Sheng LIU , Wen Xing ZHANG , Chang Qin MA , De Hua JIANG
2002, 13(6): 583-586
[Abstract](479) [FullText HTML] [PDF 56KB](1)
Abstract:
With a heptadentate compartmental Schiff-base ligand H3L (1, 3-di[o-(salicylimino) phenoxyl]-2-propanol), a new binuclear diuranyl complex [(UO2)2L(OH)]·;3DMF, C38H45N5O13U2,was synthesized and the crystal structure was determined by X-ray diffraction techniques. The coordination geometry are two pentagonal bipyramids. In each pentagon four kinds of U-O (phenoxido, hydroxo, alkoxo and ether oxo) bonds are discussed.
Synthesis and Characterization of a Novel Compound SnDy2O4
Yong ZHANG , Ke Li ZHANG , Man Ke JIA , Hao TANG , Ju Tang SUN , Liang Jie YUAN
2002, 13(6): 587-589
[Abstract](553) [FullText HTML] [PDF 24KB](0)
Abstract:
A new phase, the rare earth complex oxide SnDy2O4 was synthesized by the thermal decomposition of its oxalate precursor that was prepared by rheological phase reaction method.TG, IR, XRD and EPS were used to prove the formation of the compound SnDy2O4. The structure of SnDy2O4 was refined by Rietveld analysis. SnDy2O4 is cubic, a=7.40366Å, V=405.82Å3, Z=4.
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