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Table of Content

    24 March 1988, Volume 9 Issue 3
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    Articles
    Studies on the Preparation and Structure for Lanthanide Chloride With Dimethyl Sulfoxide
    Xie Gaoyang, Zhang Zhen, Wang Boyi, Wu Jianhua, Zheng Peiju, Gu Yidong(Yih-Tong Ku)
    1988, 9(3):  207-212. 
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    The preparation of a number of complexes of LnCl3(Ln = Nd,Sm,Eu,Gd,Dy, Tb, Er and Yb) with dimethyl sulfoxide is reported.The structures of some of them have been elucidated on the basis of infrared spectra,nmr spectra, thermoana-lysis, X-ray diffraction and chemical analysis.It appears that sulfur is the donor atom in all cases reported.From the results of single crystal X-ray diffraction analysis,it shows that the cell parameters for the species of Nd and Tb are.α= 9.7998, b= 10.1458, C=14.7505 α = 93.0376, β= 100.2652, γ = 99.6542; α= 9.7083, b = 10.1216, c = 14.6725 α = 93.3927, β = 99.8257, γ = 100.1570 respectively.Both of them are triclinic.The structure for Nd species is proposed as a distorted triangle dodecahedron.There are two lanthanide ions, ten DMSO, eight water molecules and six chloride ions in each cell.All the DMSOare coplanar and coordinated with Ln ion through oxygen atom.Among the eight water molecules, six of them are coordinated with center ions, the other two and six chloride ions are in orderly state.
    The Synthesis and Characterization of Cr(β-Dik)Cl2(β-Pic)2 Type Mixed Ligand Coordination Compounds
    Chen Ke, Luo Huimin
    1988, 9(3):  213-218. 
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    Five new mixed ligand coordination compounds with general formula Cr(β-dik)Cl2(β-pic)2 have been synthesized.The abbreviation β-dik represents acetylacetone, benzoylacetone, dibenzoylmethane, trifluroacetylacetone, thenoyltriflu-roacetone respectively; The abbreviation β-pic represents β-picoline.These coordination compounds are charecterized by using UV spectra, IRspectra and thermal analysis.
    Study of the Synthesis and the Acidity of Containing Boron Tz-01 Type Molecular Sieve
    Wang Jingzhong, Pan Lurang, Li Hexuan
    1988, 9(3):  219-223. 
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    B-Si-Al Tz-01 type molecular sieve was synthesized in a Na2O-Al2O3-H3BO3-SiO2 tartaric acid-H2O system.The ternary crystallization area of the reaetion mixture was obtained.Temperature-programmed desorption wa.s used to investigate the acidity of Tz-01 type molecular sieve.
    Study on the Solution Equilibrium of 7-(2-Pyridylazo)-8-Hydroxy quinoline
    Tong Shenyang, Zeng Wei
    1988, 9(3):  224-229. 
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    The dissociation constants of PAOx were determined spectrophotometrically in the presence or absence of surfactants.The state of PAOx in aqueous solutions was studied by using spectrophotometric and quantum chemical methods.The tautome-tric equilibrium is shifted to the quinone-hydrazone form in the presence of CTMAB.
    Synthesis of Di-p-Isopropylphenyl Sulf oxide and Study on It's Separation and Extraction Behavior by Paper Chromatography
    Xu Xiaowen, Li Lingying, Gao Dongjun, Xiao Zhenpin
    1988, 9(3):  230-233. 
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    In this paper di-p-isopropylphenyl sulfoxide (PlPSO) was first synthesized by Friedel-Crafts reaction.The elemental composition and the structural characteristics of this suifoxide were determined by elemental analysis, 1H NMR, 13CNMR, and IR.It's UVspectrum and TLCbehavior were also investigated.It's extraction behavior to more than 40 metallic ions in both HCl and.HNO3 systems were observed by reversed paper chromatography.It could be used as a stationary phase in the reversed paper chromatography successfully to separate some metal ion couples, such as Au-Pd, Au-Ag, Au-Pt, Au-Tl, Os-Ru, Os-Ir, Zr-Hf, Mo-W and others.
    Studies on the Relationship Between the Si-H Stretching Vibration arid Molecular Structure
    Zhou Xiuzbong, Geng Bolin, Wang Yoajtai, Xu Shansheng
    1988, 9(3):  234-238. 
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    The relationship between the Si-Hstretching vibration and the electronic steric effect of substituents on Si atom was studied for 19 mono-hydrosilanes (9 cyclic and 10 open chain mono-hydrosilanes).The results show that, (1) The Si-Hstretching vibration frequency is directly proportional to electronic withdrawing ability of substitucnis on Si atom in monohydrosilanes studied.Two excellent linear relationships between the Si-Hstretching vibration frequencies and Hammett substituent constants are obtained.(2) Two excellent linear relationships between the Si-Hstretching vibration frequencies and Taft substituent constants in mono-hydrosilanes are also found.(3) Areasonable mell cd of studying he electronic, steric effect of substituents on Si atcrr.s among the cyclic monohydro-tsilanes is proposed.
    Preface
    Studies on Acyl Thiosemicarbazides and Related Heterocycles (Ⅴ)——Syntheses of 1-lsonicotinoyl-4-Aryl Thiosemicarbazides and Related Nitrogen, Sulfur, Oxygen 5-Membered Heterocycles
    Zhang Ziyi, Yang Kexin, Zeng Fuli
    1988, 9(3):  239-245. 
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    1-Isonicotinoyl-4-aryl thiosemicarbazides,(Ⅰ), synthesized by the addition reactions of isonicotinoyl hydrazinc with several aryl isothiocyanates, cyclized in the presence of base, acid, or mercuric salt, and the derivatives of 1, 2, 4-triazoline-5-thione (Ⅱ), 1, 3, 4-thiadiazole (Ⅲ) and 1,3,4-oxadiazole (Ⅳ) were obtained, respectively.Preliminary experiment showed that the compounds (Ⅰ) have great promoting effect on plant (wheat, cucumber etc.) growth.
    Articles
    Studies on Cp2TiCl2-LiAlH, System——Reduction of 1,n-Diphenyl-1,n-dioles, Dibenzoylmethane, Benzoylacetone and Other Oxygen-Containing Functional Groups
    Wu Shaozu, Mizuno Kazuhiko, Otsuji YoShib
    1988, 9(3):  246-249. 
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    1,n-Diphenyl-1,n-diols, dibenzoylmethane, benzoylacetone and other oxygen-containing, functional groups undergo reduction by LiAlH4 in the -presence of Cp2TiCl2 catalyst.Thus present reaction provides a convenient way for replacing oxygen-containing functional groups at benzylic position by hydrogen.
    Studied E-t Graphs and Curves of Changing Concentrations in B-Z Reaction of Mn Catalyst
    Zhao Lianqing, Chen Zhirong, Hua Tianwei, Liao Chaoying
    1988, 9(3):  250-254. 
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    In this paper, the Mn2+ and Br- oscillating behaviour of the system were studied by using the E-t graphs, we find that both Mn2+, Br- curves in the phase plane that can not be explained by limit cycle of two-dimensions.We used xy recorder, so that projections of limit cycles were got.The dimensions ofoscillating behaviour are not less than 3.We suggest the mechanism of reaction, and give a model as oregonator.
    Intrinsic Reaction Coordinate Method in Chemistry Reaction (Ⅲ)——IRC Approach to Trans-lsomerization of Thioformaldehyde
    Li Xuekui, Sun Chiachung
    1988, 9(3):  255-257. 
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    In this paper, trans-isomerization of thioformaldehyde is studied by means of intrinsic reaction coordinate (IRC) method.The theoretical results of transition state and the normal coordinates are presented.The geometry optimization of the reactant, the transition state and the tracing of IRChave been performed by using the energy-gradient method with the split-valence 4-31G basis set
    The Dissection of Quantum Chemistry for Electronic Spectra of Phthalocyanine and Eight-x-Phthalocyanine
    Chen Qiong, Wang Guanghuai
    1988, 9(3):  258-261. 
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    Theπ electronic construction of the phthalocyanine and eight-x-phthalo-eyanjne (x means N, Satoms) has been studied by means of both group theoryand HMO methods.The "spectral contraction" phenomenon of above compoundshave been explained frpm the results of group theory disposition and Computation.
    Molecular Species Distributions of Methylolderivatives of Polyamine Compounds
    Liu Fengqi, Zheng Fuan, Tang Xinyi
    1988, 9(3):  262-267. 
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    An equation regarding molecular species distributions of the mcthylolderivativcs of polyamine compounds has been derived by the probability method in terms of one-shell substitution effects.The relationship between probabilities of generating various methylolderivatives and kinetic paramenters describing the substitution effects in initial stage and in equilibrium state of the amino-formaldehyde reaction has been obtained.The results based on the theoretical equations are good in agreement with experimental data.
    Kinetics of the Ziegler-Natta Polymerization of 1-Octene(Ⅱ)——Kinetics and Mechanism of the Induction Period
    Fan Zhiqiang, Feng Linxian, Yang Shilin
    1988, 9(3):  268-273. 
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    Kinetic curves of the polymerization of 1-octene on Solvay TiCl3-AlEt3(or Al(i-Bu)3, AlEt2Cl) catalysts were determined by dilatometer, and the induction periods during which the rate increases gradually were studied.The durations of induction periods were found to decrease with increasing[TiCl3], [M]0 and with raising temperature.The breaking of the large TiCl3, particles into small particles during the induction period was observed through a microscope.Amechanistic model was suggested which ascribes the rate increasing to the breaking of catalyst particles under the effects of the formed polymer,and the model was checked with kinetic data.
    Studies on the Synthesis, Structure and Properties of Cobalt Aluminophosphate Molecular Sieve
    Han Shuyun, Lu Dexin, Zhou Caiju
    1988, 9(3):  274-276. 
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    Cobalt Aluminophosphate (CoAPO-5) molecular sieve was synthesilzed by hydrothermal method.The crystal structure of CoAPO-5 has been studied by X-ray diffraction, electron probe-and infrared spectra.The parameters of the unite cell and chemical composition of CoAPO-5 have been determined.Some properties of CoAPO-5 such as adsorption isotherms, thermal stability, acidity have been investigated.These results illustrate that cobalt enter the framework of CoAPO-5 molecular sieve.
    An Investigation on the Metal Decavanadates Coordinating with Oxine (Ⅲ)——The Synthesis, Characterization and Properties of Lithium, Potassium and Ammonium Salts
    Du yaoguo, Wang Jun, Wang Xiaoxia, Xiu Zhenkun, Du Wencai
    1988, 9(3):  277-279. 
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    The decayahadates of Li+,K+,NH4+ coordinating with oxine were prepared.By means of elementary analysis, molecular weight determination, GC/MS, X-rays diffraction, UVand IRspectrophotographies and thermo-analysis, the authors suggested that the structural formulae of Li+,K+,NH4+ salts are as follows:[Li(HOx)]2[Li(HOx)3]4(H2V10O28(Ox)2]·4HOx,[K(HOx)]4[K(HOx)2]2[H6V10O28(Ox)6]·2HOx,and [NH4(HOx)]4[NH4(HOx)2]2[H4V10O28(Ox)4.
    Synthesis and Characterization of Solid Complexes of Scandium and Yttrium Perchlorates with 1,8-Naphthyridine-N-Oxide
    Gan Xinmin, Tan Minyu
    1988, 9(3):  280-282. 
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    The solid complexes of scandium and yttrium perchlorates with 1, 8-naphthy-ridine-N-oxide (napyo) having the.compositions Sc(napyo)4(ClO4)3 and Y(napyo)4(ClO4)3 have been synthesized, in methanpl medium.The new complexes have been characterized by elemental analysis, IRspectra, molar conductance, differential thermal analysis (DTA) and thermograyimetry (TG).
    Preface
    Syntheses of 1-Benzothiazolylthioacetyl-4-Arbylthi-osemicarbazide Compounds
    Chen Limin, Zhang Ziyi, Zhang Xian, Cai Dongxian, yuan Dong
    1988, 9(3):  283-286. 
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    The interaction of equimolar quantities of benzothiazolylthioacetyl hydrazin(Ⅴ) and aroylisothiocyanates in dry acetone yields a Series of new 1-benzothia-zolylthioacetyl-4-aroylthiosemicarbazides(Ⅵ):  The structures of all the compounds synthesized were characterized byelemental analyses, infra-red spectra and by nuclear magnetic resonance spectraand mass spectra for some representative compounds.The determination ofbiological activity of all the compounds is going on.
    Articles
    Studies on Polarographic Adsorption Wave of Dibromopiaselenole and Its Application
    Cai Qiantao, Shi Wenzhao
    1988, 9(3):  287-289. 
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    In this paper the polarographic behaviour and mechanism of adsorption wave of 4,6-dibromopiaselenole(4,6-diBr-PIS) in several mediums are studied by cyclic voltammetry and differential neopolarography.In weak acidic medium 4,6-diBr-PlSgave a sensitive irreversible adsorption wave (Epc = -0.1Vvs.AgCl/Ag electrode) on mercury electrode.The wave could be used as basis of the sensitive semi-differential neopolarographic method for the determination of trace selenium.
    The Gas-Solid Bromination of Bipheriyl in the Presence of β-Cyclodextrin
    Huang Naiju, Guo Qing, Zhang Daodao
    1988, 9(3):  290-291. 
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    The gas-solid bromination of biphenyl in the presence of β-cycled extrin has been studied.The experimental data indicated that the rate of consumption of biphenyl in the presence of β-cyclodextrin is ten times greater than that when no β-cyclodextrin is present.lt was found that this reaction has high para selectivity.
    Studies on Flavonoids (Ⅵ)——Synthesis of the 8-Bromo-4′,7-Dihydroxyisoflavone
    Yue Baozhen, Gu Songli, Cai Monshen
    1988, 9(3):  292-294. 
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    8-Bromo-4′ 7-dihydroxy isoflavone(Ⅴ) was synthesized from 2-bromorecercinol (Ⅱ).Debromonation occurs unexpectedly by using BF3-ether as Lewis acid in F.Creaction between Ⅱ and p-methoxy-phenylacetic acid.Demethoxylation of 3-brpmo-2,4-dihydroxy,4′-methpxy .deoxybenzoin(Ⅲ) was carried out in CH3CN at - 10℃ with excess of BBr3 (1:10mol).3-bromd-2,4,4′-trihydroxydeoxybenzoih(Ⅳ) was cyclized with N,N-dimethyl formamide dimethyl acetal to give Ⅴ,and a by product, 4′,7-dimethoxyisoflavone, was also isolated, Ⅳ was also prepared by the direct bromination of 2,4,4′ -trihydroxydepxybenzoin.
    The Synthesis of 1-Aminocyclohexyl Phenyl Phosphonates and 1-Cyclopropyl Phosphonates
    Chen Ruyu, Liu Zengxun, Chen Linzhi
    1988, 9(3):  295-297. 
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    In this paper the synthesis of four new 1-amino cyclohexyl phenyl phospho-nic acids was reported.Two new intermediates "Pyrazoline" were prepared by the addition of diazomethane to the substituted olefins.After the elemination of nitrogen by heating, the substituted cyclopropyl phosphonates were obtained in good yields.
    A Program Plotting Molecular Orbitals for the Ab Initio Calculations
    Shen Erzhong, Wang Zhizhong, Jiang Yuansheng
    1988, 9(3):  298-300. 
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    Aprogram plotting molecular orbitals for the ab initio calculations using STO-NG basis set is reported in this paper.The program can used to draw the stereograms and their sectional maps of the computed atomic or molecular orbitals.As an example, we have shown some diagrams for the Hand C6H6.
    The Potential Oscillation During Anodic Dissolution of Iron in Concentrated NaCl Media
    Wang Xuelin, Nobe Ken
    1988, 9(3):  301-303. 
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    The galvanostatic potential oscillations during anodic dissolution of iron in concentrated chloride media were investigated.The minimum currents which caused the oscillations were observed.The periods of oscillations were affected by the rotation rates of the electrode, electrolyte concentration and current densities.It was considered that the form and dissolution of FeCl2 and Fe(OH)2 film were the cause of potential oscillations.For the oscillations with stationary electrode, the imposed current densities were inversely proportional to the square root of the periods, which was consistent with the result by analysing the diffusion equation.
    Studies on the Formation Temperatures of Si3(PO4)4 and Acid Ratio of P2O5/SiO2 Catalysis
    Han Weiping, Zhao Zheng
    1988, 9(3):  304-306. 
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    The phase formation of Si3(PO4)4 for P2O5/SiO2 catalysts has been investigated by XRD, reaction chroma tography and amine adsorption.The results showed that the 400~500℃ is important range of phase formation, if the calcination temperature below them, with the increase of temperature, the crystallinity and crystallite size will be advance, if the temperature higher than this range, such as 500~800℃, the crystallinity and crystallite size retain constants.As it happens, it can be found from the variations of DMDO delivery volume and surface acid concentration, there are indicated turning points in 400~500℃.But also the relative surface area of crystal phase of Si3(PO4)4 and relative yield of isoprcne reach maxmarn within the range of temperatures 500~800℃.The reasons for the adhesion between catalyst particles arc also explained.
    Crystal and Molecular Structure of N1-Acetyl-N3-O-Toluyl -5-Fluorouracii
    Jiang Anbei, Hu Shengzhi, Wang Yikang, Chen Qi
    1988, 9(3):  307-309. 
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    The crystal of the title compound belongs to monoclinic system.Space group P21/n, with dimensions.α = 15.795(4), b = 8.367(3), c = 10.720(4) Å,β = 104.98(3)o, V= 1368.6Å3,Z= 4, Dc = 1,409gcm-3, μ(MoKα) = 1.067cm-1, λ(MoKα) = 0.71069 Å.The final R/Rw = 0.045/0.039 for 235 parameters and 1898 observed refledions were Treasured with an FNRAF-NONIUS CAD-4 diff-ractometer using MoKα radiation at 293K.The molecule consists of fluorouracil moiety and o-toluyl group which are virtually perpendicular to each other.The present paper deals with brief discussion of the structural features which may be responsible for its special antitumor activity for the title compound.
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