1999 Volume 10 Issue 11

Asymmetric Photocatalyzed Addition of Cyclic Ammes to the Chiral 5-(l)-Menthyloxy-2(5H)-furanone
Zhao Yang WANG , Tian Ying JIAN , Qing Hua CHEN
1999, 10(11): 889-892
[Abstract](310) [FullText HTML] [PDF 126KB](0)
The benzophenone-initiated photoaddition of N-methyl amines 2 to the chiral synthon 1 proceeds in a regiospecitic and highly stereocontrolled fashion to give the C-C photoadducts containing a newly stereogenic center 3a-3c.The enantiomerically pure N-C photoadducts, amino butenolides 5a-5c have been obtained from the enantioselective photoaddition of secondary cyclic amines 4 with the chiral synthon 1 under the same conditions.
Bimolecular Self-Condensation of Pyrrolizinones Induced by Grignard Reagent
Wen Ge YAN , Shou Fang ZHANG , Li Jun WU
1999, 10(11): 893-894
[Abstract](210) [FullText HTML] [PDF 75KB](0)
The products of pyrrolizinones with 3-methoxyphenyl magnesium bromide were bimolecular condensation compounds, not the related alcohol, and they, were confirmed by IR, 1H-NMR, 13C-NMR, HMQC, HMBC, NOE-differ., MS and Elemental Anal.This indicated that Grignard reagent is a catalyst here.
The Influence of Ketones on the Formation of Symmetrical Secondary Amine:A New Method for Preparation of N, N-Bis-(dimethoxyphenylethyl)amine
Chong Zhao RAN , Lin XIA , Pei Zhou NI
1999, 10(11): 895-898
[Abstract](215) [FullText HTML] [PDF 113KB](1)
The influence of some ketones on the formation of symmetrical secondary amine N.N-bis-(3.4-dimethoxyphenylethyl)amine 1 were discussed and a new method for preparing 1 was described.
Reductive Cleavage of S-S Bond by Sm/NiCl2 or Sm/NiCl2·6H2O System:A New Method for the Preparation of Thiolesters
Hua Yue WU , Red Er CHEN , Yong Min ZHANG
1999, 10(11): 899-902
[Abstract](216) [FullText HTML] [PDF 121KB](0)
Disulfides were reduced by the Sm/NiCl2, or Sm/NiCl2·6H20 system to generate thiolate anion.which reacted further with anhydrides or acyl chlorides to afford thiolesters in good yields under mild and neutral conditions.
Synthesis of 3 or 4-Substituted Pyridine-2, 6-Dicarboxylic Acid
Xian Hong YIN , Man Ya YANG , Hua Hong SHI , Lian Quan GU
1999, 10(11): 903-906
[Abstract](343) [FullText HTML] [PDF 126KB](0)
Various 4-alkoxypyridine-2, 6-dicarboxylic acids were synthesized starting from 2, 6 lutidine.Through aldol condensation and Michael addition, various 4-arylpyridine-2, 6 dicarboxylic acids were synthesized starting from aromatic aldehydes and 2-acetylfuran.
Synthesis of Isoquinoline-1, 3-Dicarboxylic Acid
Xian Hong YIN , Man Ya YANG , Hua Hong SHI , Lian Quan GU
1999, 10(11): 907-910
[Abstract](217) [FullText HTML] [PDF 130KB](2)
Two new compounds, isoquinoline-1, 3-dicarboxyaldehyde and (IDA) were synthesized via 6 or 7 steps starting from benzaldehyde, or prepared via 4 steps starting from allylbenzene.
A Facile Synthsis of ω-Bromo-Diene Via Solid/LiquidTransferred Wittig Reactions of ω-Bromobutyltriphenylphosphonium Salts With α.β-Unsaturated Aldehydes
De Qing SHI , Ru Yu CHEN
1999, 10(11): 911-914
[Abstract](289) [FullText HTML] [PDF 130KB](2)
A new approach to the synthesis of ω-bromo-dimes was carried out by using solid/liquid transferred Wittig reactions between ω-bromobutyltriphenylphosphonium salt and α.β-unsaturated aldehydes.
The Synthesis of Gallic Esters of Higher Fatty Alcohols under Solvent-Free Conditions Using Microwave Irradiation
Hai Xia LIN , Li Xue Zhang , Liang Shi CHENG
1999, 10(11): 915-916
[Abstract](216) [FullText HTML] [PDF 81KB](0)
The reactions of gallic acid with higher fatty alcohols are accelerated by microwaves under solvent-free conditions in the presence of p-toluenesulfonic acid to afford a high yield synthesis of higher fatty alcohol gallates.Montmorillonite K 10 are less efficient.
Synthesis of 1, 7-Bis(4-hydroxyphenyl)-3-hydroxy-1, 3-heptadien-5-one
Ming Zhao ZHU , Shao Bat LI , Qiang GAO , Guo Lin ZHANG
1999, 10(11): 917-918
[Abstract](198) [FullText HTML] [PDF 71KB](0)
A facile synthesis of the analog of curcumin, 1, 7-bis (4-hydroxyphenyl)-3-hydroxy-l, 3-heptadien-5-one 1 was achieved.The key step, was completed through the regioselective condensation of ketone 5 and acyl chloride 7.
Two Quinones from the Aerial Parts of Sphallerocarpus gracillis
Neng Yu CHEN , Jun SHI , Tao CHEN
1999, 10(11): 919-920
[Abstract](175) [FullText HTML] [PDF 83KB](0)
Two new quinones were isolated from the aerial parts of Sphallerocarpus gracillis Their structure were determined by snectrosconic methods (HRMS, 2n NMR) and finally confirmed by X-ray crystallography.
Vaccariside A, Novel Saponin from Vaccaria segetalis (Neck.) Garcke
Ji MA , Wen Cat YE , Hou Ming WU , Fa Hu HE , Jing Zhen DENG , Shou Xun ZHAO
1999, 10(11): 921-924
[Abstract](179) [FullText HTML] [PDF 187KB](1)
A new triterpenoid saponin, vaccariside A 1 was isolated from the seeds of Vaccaricr segetalis using various chromatographic methods.The structure of compound 1 was elucidated by comprehensive spectroscopic analysis as 3-0-p-D-galactopyranosyl-(1-2)-[B-D-quinovpyranosyl-(1-4)-B-D-xylopyranosyl-(1-3)]-(3-D-glucuronopyranosyl quillaic acid 28-0-B-D-glucopyranosyl-(1-3)-B-D-xylopyranosyl-(1-A)]-a-L-rhamnopyranosyl-(1-2)-3-O-acetyl-B-D-fucopyranoside.
A Pair of New Geometrically Isomeric Triterpenoid Saponins from the Seeds of Aesculus chinensis
Xiu Wei YANG , Jing ZHAO , Yu Xin CUI , Li He ZHANG
1999, 10(11): 925-928
[Abstract](176) [FullText HTML] [PDF 134KB](0)
Two new triterpenoid saponins were isolated from the seeds of Aesculus chinensis by preparative HPLC.On the basis of chemical evidence and spectral data, their structures were established as 21β-tigloyl-28-acetylprotoaescigenin 3β-0-[β-D-xylopyranosyl (1→2)] [β-D-glucopyranosyl (1→4)]-β-D-glucopyranosiduronic acid (isoescin Ⅱa, 1) and 21β-tigloyl-28-acetylprotoaescigenin 3β-0-[β-D-xylopyranosyl (1→2)] [β-D-glucopyranosyl (1→4)]-β-D-glucopyranosiduronic acid (isoescin 11b, 2), which are a pair of geometrical isomers.
Small Peptide Interacting with Pollen Calmodulin and their Effects on Cellular Functions
Jing SU , Yan Ling SONG , Min HU
1999, 10(11): 929-932
[Abstract](187) [FullText HTML] [PDF 181KB](0)
The interaction between dansyl-labeled pollen calmodulin (D-pCaM) and synthesized peptides was studied in the presence of Ca2+ by fluorescence spectra.It is found that Gly/L-Ala→D-Ala substitution in peptide chains caused great changes in their affinity for pCaM.Besides.our data provided evidence on the dissimilarity of different Calls although they have highlyconserved structures.A preliminary study was carried out on the effects of CaM-binding peptides on cellular signal transduction, cell proliferation, showing the participation of CaM in cell functions mentioned above.
Direct Enantiomer Separation of 2-Phenylcyclopropanecarboxylate Esters on Cyclodextrin Derivatives Stationary Phases in GC
Meng Yan NIE , Liang Mo ZHOU , Xue Liang LIU , Qing Hai WANG , Dao Qian ZHU
1999, 10(11): 933-936
[Abstract](177) [FullText HTML] [PDF 135KB](0)
Direct enantiomeric separation of all four optical isomers of 2-phenylcyclopropane carboxylate ester was first achieved on each of the three differentp-cyclodextrin chiral stationary phases (CSPs) in GC.Using these CSPs, enantiomeric excess of the products of enantioselective cyclopropanation can be determined directly, conveniently and fast.
Ground State Spins of Bicarbcnes and Binitrenes, Coupled through Electron-Rich Rings
Hai Quan HU , Yong Jun LIU , Da Cheng FENG , Cheng Bu LIU
1999, 10(11): 937-940
[Abstract](180) [FullText HTML] [PDF 112KB](0)
The ground state spins coupled through electron-rich rings of bicarbenes and binitrenes have been studied at UHF/6-31G* level. The results demonstrate that ferromagnetic coupling exists in these molecules, and electron-rich rings are the potential ferromagnetic coupling units.
Jahn-Teller Effect on Binary Indium Bromide ─An Ab Initio Study
Ke Chen WU , Jun LI
1999, 10(11): 941-944
[Abstract](259) [FullText HTML] [PDF 140KB](0)
In order to elucidate the unusual chemical sensitivity of binary indium bromides.the potential energy surface of the model complex InBr87- has been-studied by means of ab initio allelectron calculation with larger basis sets.The configuration is on a local maximum of the energy surface and crystal potential around In+ is soft, allowing small spontaneous distortions as a result of a second-order Jahn-Teller instability.
Electrochemical Reduction Characteristics of α-Nitronaphthalene in Sulfuric Acid Solution
Chun An MA , Wen Km ZHANG , Yong Ping GAN , Hui HUANG , Mei Chao LI , Shao Ping TONG
1999, 10(11): 945-948
[Abstract](273) [FullText HTML] [PDF 128KB](0)
The electrochemical reduction characteristics of α-nitronaphthalene in sulfuric acid solution were first reported in this paper.The results showed that the 1-amino-5-naphthol can be prepared by electrodeduction from α-nitronaphthalene and reduction peak corresponding to the reaction of α-nitronaphthalene to 1-amino-5-naphthol was in the range of-0.40~0.60V(vs.D.H.E) on the amalgamated copper cathode in the presence of SnCl2 additives.The mechanism of α-nitronaphthalene electroreduction to 1-amino-5-naphthol was also investigated.the overall electroreduction reaction was composed of two intermediate steps and two intermediate products existed in solution.The electrochemical reduction mechanism was similar to that of nitrobenzene to para-aminophenol.
Synthesis and Spectrophotometric Studies of 2-(2-Imidazolylazo)-5-Dicthylamino Phenol
Fu You PAN , Chang Hua GE , Hua Ding LIANG
1999, 10(11): 949-952
[Abstract](177) [FullText HTML] [PDF 139KB](0)
In this paper, 2-(2-imidazolylazo)-5-diethylamino phenol (IZAPN) was prepared, the protonation behaviour and the condition of spectrophotometric determination of cobalt with this reagent are reported.The results show that the new colour reagent reacts with cobalt to from a stable purple red complex (1:3). However, the complex formed could be changed into another species with stable absorptivity by addition of mineral acid (1+1).The.method is highly selective and sensitive and has been applied to the direct determination of cobalt in some alloys with satisfactory results.
Synthesis and Fluorescence Quenching of Copolymer Containing 3, 4, 9, 10-Perylenetetracarboxyl Diimide Side Chains
Zhao ZHANG , Zhao Bin CHEN , Feng Lian BAI , Yue Ping ZHANG , Yi Ming MO , Min ZHEN , Xiao Lin YAN , Yu hang LI
1999, 10(11): 953-956
[Abstract](187) [FullText HTML] [PDF 128KB](0)
A photoluminescence material, copolymer of N-vinylcarbazole(VCz)and N, N'-bisallyl-3, 4, 9, 10-Perylenetetracarboxyl diimide (APTC) chromophores P(VCz-APTC) was synthesized.The fluorescence quenching of P(VCz-APTC) by fullerene (C60) and triethylamine was also studied.
Spectrophotometric Investigation of Cadmium Complex Solution with m-Bromobenzenediazoaminoazobenzene
Hong Wen GAO , Lei WANG , Hao YE
1999, 10(11): 957-960
[Abstract](255) [FullText HTML] [PDF 169KB](2)
The synthesis of a new ligand, m-bromobenzenediazoaminoazobenzene (m-BBDA) was carried out.The reaction between m-BBDA and cadmium(Ⅱ) was sensitive at pH over 12 and in the presence of emulsifier OP.Because of the high interference of excess of ligand β-correction theory was applied instead of the single wavelength method. This study gave the simple determination of the complex ratio, real molar absorptivity(ε)and step or cumulative stability constant (K).
Intrachain and Interchain Interactions in Polystyrene:Dilute and Semidilutc Solutions
Xin Song LI , Guo Chang WANG , Bing Lin HE
1999, 10(11): 961-964
[Abstract](186) [FullText HTML] [PDF 186KB](0)
Excimer formation in pyrenyl labeled polystyrene has been investigated in dilute solution region.The change of the intensity ratio of excimer to monomer (Ie/Im) with increasing concentration(C), is interpreted by intrachain and interchain interactions.The double logarithmic plot of Ie/Im vs C displays two critical points, Csat about 2.5×10-3g/ml and C+ at about 3.2×10-2 g/ml.In dilute region Cs, excimer formation may be controlled by intrachain interaction.
The Effect of Neodymia on the Activity of Hydrocarbon Synthesis Catalysts from Carbon Dioxide
Xin Ying LIU , Guo Cai DENG , Yun Ti CHEN
1999, 10(11): 965-966
[Abstract](183) [FullText HTML] [PDF 85KB](0)
In this paper, neodymia was added into hydrocarbon synthesis catalysts by solidmixing method to improve the activity of hydrocarbon synthesis catalyst from carbon dioxide.0.1% Nd2O3 can improve the carbon dioxide conversion and light olefin selectivity at 523 and 573K.but decrease the activity at 623K.
Effect of CeO2 Promoter on the Performance of Catalyst for CH4, CO2with O2 to Synthesis Gas
Li Yong FU , Qun Biao WANG , Shao Jie LU , Wei Guo XIE , Fa Li QIU
1999, 10(11): 967-970
[Abstract](172) [FullText HTML] [PDF 136KB](0)
In the reaction of methane, carbon dioxide with oxygen to synthesis gas, conversion of CH4 was increased, but CO selectivity was reduced when CeO2 was added to Ni/Ca0-Al2O4 catalyst.The characterization of TPR, XPS, XRD and H2-TPD exhibited that, on one hand, the CeO2 promoter decreased the reduction temperature of catalyst.On the other hand, addition of CeO2 resulted in an increase in the electron density of active component Ni, and as a result, reduced the ability of CH4 deep cracking and enhanced the resistance to carbon-deposition of catalyst.In addition; the existence of CeO2 was beneficial to decrease the Ni crystal particle size.
Synthesis, structure and spectroscopic properties oforganophosphoryl polyoxotungstates of Formula α-[R2PW9O34]5-(R=C6H5P(S), C6H11P(O))
Zhen Gang SUN , Jian Xin LI , Qun LIU , Jing Fu LIU
1999, 10(11): 971-972
[Abstract](179) [FullText HTML] [PDF 107KB](0)
Tetrabutylammonium salt of organophosphoryl derivatives of trivacant tungstophosphate of formula a-[R2PW9O34]5- (R=C6H5P(S), C6H11P(O)) have been prepared, purified and characterized by elemental analysis, IR, 31P and 83W NMR.According to spectroscopic observations and chemical analysis, the hybrid anion consists of an α-[PW9O34]9- framework on which are grafted two equivalent organophosphoryl groups through P-O-W bridges, and the IR spectral data show that these new species still retain the keggin structure.
Reaction of [(μ-RE)(μ-CO)Fe2(CO)6]-[Et3NH]+ (E=S, Se, Te) Salts with Benzenesulfinyl Chloride and Carbon Disulfide
Chao Guo YAN
1999, 10(11): 973-974
[Abstract](177) [FullText HTML] [PDF 103KB](0)
The salts of[(μ-RE)(μ-CO)Fe2(CO)6]-[Et3NH]+(E=S, Se, Te) react with bcnrenesulfinyl chloride to dive the μ-sulfinvl croup brideed complexes(μ-RE)(μ-PnS=O)Fe2(CO)6 in goon yeias.Wnereas the sans [(μ-RS)(μ-CO)Fe2(CO)6)-[Et3NH]+(R=t-Bu, Ph) react with carbon disulfide to yield the dithioformato-brideed anionic salts [(μ-RS)(μ-S=C-S)Fe2(CO)6)-[Et3NH]+, wmcn react in situ at tne exo-suuur atom of the ditmorormato-group with diverse α,β-unsaturated carbonyl compounds to give Michael addition products in moderate yields.
The Assembly and Molecular Structure of a Novel One-dimensional Cyanide-bridged [Ni(pn)2Ni(CN)4]n·nH2O Complex
Xiu Ying ZHANG , Dong GUO , Jun Ming TANG , Shu Zhong ZHAN , Qing Zi HAN , Chen Xia DU , Yu ZHU , Rui Na YANG
1999, 10(11): 975-978
[Abstract](171) [FullText HTML] [PDF 166KB](0)
The synthesis, structure and characterization of a new one-dimensional cyanide-bridged complex [Ni(pn)2Ni(CN)4]n·nH2O (where pn=1,2-diaminopropane) are described.The structure of this complex consists of a one-dimensional polymeric chain-Ni(pn)2-NC-Ni(CN)2-CN-Ni(pn)2-in which the Ni(Ⅱ) centers are linked by two CN groups.
Synthesis of Mesoporous Silica Molecular Sieves via a Novel Templating Scheme
Xiao Ming ZHANG , Zhao Rong ZHANG , Ji Shuan SUO , Shu Ben LI
1999, 10(11): 979-982
[Abstract](181) [FullText HTML] [PDF 267KB](0)
Mesoporous silica molecular sieves have been synthesized under mild conditions by using in situ prepared N, N-dimethyldodecylamine oxide as template.
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