中国化学快报

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THE RADICAL NUCLEOPHILIC SUBSTITUTION REACTION OF HETEROCYCLIC KETENE AMINALS WITH 2, 4-DINITROHALOBENZENES

Wen Yi ZHAO, Zhi Tang HUANG

中国化学快报. 1991, 2(07): 501-504.

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The anion of heterocyclic ketene aminals 1 reacted with 2, 4-dinitro-halobenzenes 2 to give an arylated product 3 through the radical nucleophilic substitution confirmed by ESR spectroscopy, ESR-spin trapping technique, and depression of the reaction rate by the addition of inhibitor.

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REGIOSELECTIVE OXIDATION OF KETONE BY AN OXIDATIVE REAGENT SYSTEM KH/O₂/18-CROWN-6/THF:APPLICATION TO SYNTHESIS OF VARIOUS LACTONES

Wei Shan ZHOU, Biao JIANG, Xin Fu PAN

中国化学快报. 1991, 2(07): 505-508.

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the regioselectivity in the oxidation of different types of ketone compounds 1--6 with an oxidative reagent system, KH/O₂/18-Crown-6/THF is described.From these oxidative products, the various lactones have been prepared.

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A NOVEL STEROID FROM EICHHORNIA CRASSIPES

Hou Ming WU, Hui Qiang ZHOU, Sheng yu HUANG, Kan MA, Xia Fei LAO, Shu Wen YU, Wen Hao SUN, Zi Wen YU

中国化学快报. 1991, 2(07): 509-512.

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6α-Hydroxy-stigmasta-4, 22-diene-3-one 1, a novel steroid, was isolated from the Eichhornia Crassipes.Its structure was determined by ¹H and ¹³C NMR spectroscopy and further confirmed by authentic sample, which was synthesized from stigmasterol 2.

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SYNTHESIS OF 6, 7-METHYLENEDIOXY-3-THIA-1(2H, 4H)ACRIDONE AND THE RELATED THIA-ACRIDINE-PUSED HETEROCYCLIC COMPOUNDS

Ji Rui HOU, Jin Jun WANG, Gui Ji JIANG, Jing Shu LI

中国化学快报. 1991, 2(07): 513-514.

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6, 7-Methylenedioxy-3-thia-1(2H, 4H)acridone and the related acridine-fused quinolines and pyridines, and also their flavylium-perchlorates were synthesized.The structures of all these compounds prepared are characterized by elemental analysis.IR and H-NMR spectra.

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DARZENS REACTION OF 2-CHLOROMETHYLBENZOXALINE

Chao Guo YAN, Wen Xing LU, Ji Tao WU

中国化学快报. 1991, 2(07): 515-516.

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2-chloromethylbenzoxaline reacted with aromatic aldehydes in alkaline solution, giving Darzens condensation product:2-aryl-3-benzoxalinyloxiranes.

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THE APPLICATON OF ULTRASOUND TO THE DI-ALKYLATION AND CYCLO-DI-ALKYLATION OF ETHYL CYANOACETATE UNDER SOLID-LIQUID PHASE TRANSFER CONDITIONS

Qi Jun LIN, Yong Ming ZHANG, Cheng Ru ZHANG, Wen Zhen SONG, Qin QIU

中国化学快报. 1991, 2(07): 517-520.

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Comparative experiments show that ultrasonic irradiation reduces the reaction times and improves the yields in the di-alkylation and cyclo-di-alkylation of ethyl cyanoacetate under solid-liquid phase transfer conditions.

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SYNTHESIS OF 4, 5-SECOCHOLESTANE AND 4-METHYL-4, 5-SECOCHOLESTANE

Jian Guo, MA Tong Shuang, LI Yu Lin LI

中国化学快报. 1991, 2(07): 521-522.

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The synthesis of 4, 5-secocholestane and 4-methyl-4, 5-secocholestane from cholesterol are reported.

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STEREOSELECTIVE SYNTHESIS OF ACETYLATED GLYCOPYRANOSYL AZIDES

Jian Xin YU, Yu Ting LIU

中国化学快报. 1991, 2(07): 523-524.

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The acetylated glycopyranosyl azides (5-8) were obtained in high yields with stereoselectivity by phase-transfer catalyzed(PTC)synthesis, and their structures were confirmed depending upon elemental analysis and IR, ¹H, ¹³C-NMR spectral data.

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SYNTHESIS OF 4, 6-DISUBSTITUTED 5-THIOXO-1, 2, 4-TRIAZIN-3-ONE FROM BENZOTHIOFORMANILIDE

Zhong E LU, Tian Lin XU, Xiao Dong SHI

中国化学快报. 1991, 2(07): 525-526.

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A method of synthesis of 4, 6-disubstituted 5-thioxo-1, 2, 4-triazin-3-ones from benzothioformanilides and semicarbazide is described.And six new compounds were synthesized by this method.

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DIELS-ALDER REACTIONS OF FURAN WITH DIENOPHILES CATALYZED BY YbCl₃

Zi Niu ZHOU, Qi SHEN

中国化学快报. 1991, 2(07): 527-528.

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The yield and stereoselectivity of the Diels-Alder reactions between furan(or 2-methylfuran)and different dienophiles are markedly enhanced by the catalysis of anhydrous YbCl₃.

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THE SYNTHESIS AND CRYSTAL STRUCTURE OF CIS-BIS(1, 10-PHENANTHROLINE)GLYCINECOBALT(Ⅲ)

Bao Hui YE, Tian Xian ZENG, Liang Nian JI, Hong Hui ZHUANG

中国化学快报. 1991, 2(07): 529-530.

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A new coordination compound of cis-bis(1, 10-phenanthroline)glycinecobalt(Ⅲ)chloridate tetrahydrate, cis-[Co(phen)₂gly]Cl₂.4H₂O, has been prepared by glycine reacted with cis-[Co(phen)₂Cl₂]Cl, then isolated by SP-Sephadex C-25 H⁺ form column.The crystal and molecular structure of the new compound has been determined by RIGAKUAFC5R four circle diffractometer, 5032 independent reflections were collected of which 3781 observable reflections were used for structure refinement.The crystal is monoclinic, space group C2/c, with a=35.13(1) Å, b=9.637(3) Å, c=17.485(6) Å, β=115.08(2)^a, V=5362(3) Å³, Z=8.The structure was refined by full matrix least-squares procedure to a final R=0.041 and R_ω=0.060.The molecular formula was CoC₂₈H₂₈N₅O₈Cl₂.with molecular weight M_r=636.38, D_c=1.58g/cm³, μ=8.88cm^-1 and F₍₀₀₀₎=2624.

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STUDIES ON 1, 2, 3-DIAZAPHOSPHOLE Ⅳ REACTION OF 1, 2, 3-DIAZAPHOSPHOLE WITH ALCOHOLS

Bao Zhong CAI, Lun Tzu LIU, Ru Yu CHEN

中国化学快报. 1991, 2(07): 531-534.

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Rapid addition of alcohols to 1, 2, 3-diazaphosphole 1 easily gave tricoordinated phosphorus compounds, which were sulfurized to tetracoordinated phosphorus compounds.When ethylene glycol and aminoethanol were used separately to react with 1, the tricoordinated phosphorus compounds which formed, rearranged to pentacoordinated phosphorus compounds and the substituents at N₂ affected the rearrangement significantly

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THE REGIOSPECIFICITY OF INTRAMOLECULAR N-3-BUTENYL NITRONE CYCLOADDITION

Si Yu MA, Xiao Yuan FU

中国化学快报. 1991, 2(07): 535-536.

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The reaction mechanism of the intramolecular cycloaddition of N-3-butenyl nitrone has been investigated theoretically by using AM1 MO method and transition state theory.There are two parallel reactions leading to two different regioisomers.The ratio of the rate constants of these two reactions was calculated to be 124.1(at 383.75 K).The obtained results can be used to explain the high regiospecificity of the reaction product.

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AN IHSECTICIDAL SESQUITERPENE FROM CELASTRUS ANGULATUS

Mao Tian Wang, Hai Lin Qin, Yan Zi Li, Man Kong

中国化学快报. 1991, 2(07): 537-538.

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An insecticidal sesquiterpene polyol ester, angulatin A, was isolated from the root bark of Celastrus angulatus.Its structure was established as 1α, 2α-diacetoxy-8β, 15-diisobutyryloxy-9α-benzoyloxy-4β, 6β-dihydroxydihyclro-β-agarofuran by spectroscopic methods.

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TEUPERNIN A, B AND C, THREE ENT-CLERODANE DITERPENOIDS FROM TEUCRIUM PERNYI FRANCH

Di An SUN, Guang Yi LI

中国化学快报. 1991, 2(07): 539-542.

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Three furanoid ent-clerodane diterpenoids, teupernin A, B and C have been isolated from the acetone extract of Teucrium pernyi Franch.Their structures were established by spectroscopic means(UV, IR, MS, ¹H NMR, ¹³C NMR, H-H COSY, C-H COSY and NOE)and by comparison with related compounds.

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A NEW SESTERTERPENE FROM THE SPONGE PHYLLOSPONGIA FOLIASCENS

Xiong FU, Long Mei ZENG, Jing Yu SU, Francis J. SCHMITZ

中国化学快报. 1991, 2(07): 543-544.

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Phylloketal(1), a new sesterterpene which belongs to the scalarane class of sesterterpenes with a 20, 24-bishomo-tetracyclic skeleton, has been isolated from the South China Sea sponge Phyllospongia foliascens, and its structure was characterized mainly by one and two-dimensional NMR.

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THYMINE BONDED-STATIONARY PHASE FOR HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

Tao ZHU, Qin Wei WANG, Lian Zhu SHEN, Cheng Xun LU, Yi Liang SUN

中国化学快报. 1991, 2(07): 545-548.

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A new type of HPLC stationary phase containing thymine derivative was successfully prepared.It was found to give selective separation of nucleic acid bases and several purine derivatives, such as caffeine and theophylline.The retention behaviour and elution order of the solutes were interpreted in terms of molecular structure.

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THE OBSERVATION OF ENHANCED RAMAN SCATTERING OF GASEOUS MOLECULES BY Hg MICRODROPLETS

Fa Ping ZHONG, Han Xi YANG, Zhong SHI, Chuan Sin CHA, Zhi Shan Xu, Nian XIAO, Rong Sen SHEN

中国化学快报. 1991, 2(07): 549-550.

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ABSTRACT The Raman intensitics of gas molecules were found to be enormously enhanced in the presence of Hg-microdroplets.The enhancement factor for the molecules studied was found to be over 20.

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THE RAPID DETERMINATION FOR BENZO(a)PYRENE WITH SYNCHRONOUS FLUORESCENCE SPECTROSCOPY SCANNING IN DEFINED RANGE OF DUAL-WAVELENGTHS

Wei Xi YAO, Wen Xian CUI, Tao XIONG, Xiao Bai XU

中国化学快报. 1991, 2(07): 551-552.

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A rapid method of determination of BaP in various environmental samples, using synchronous fluorescence spectroscopy scanning in defined range of dual-wavelengths(SFDW)is described in this paper.

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SYNTHESIS AND STRUCTURE OF TETRANUCLEAR MOLYBDENUM CLUSTER COMPOUND[Mo₄S₄(μ-O₂CC₆H₅)₂(dtp)₄]

Hong Hui ZHUANG, Ding Ming WU, Jian Quan HUANG, Jin Ling HUANG

中国化学快报. 1991, 2(07): 553-554.

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The cluster compound [Mo₄S₄(μ-O₂CC₅H₅)₂(dtp)₄](dtp=S₂P(OEt)₂)was obtained by the ligand substitution reaction of tetranuclear molybdenum cluster [Mo₄S₄(μ-dtp)₂(dtp)₄]in the mixed solvent of acetone, ethanol and water in the presence of C₆H₅CO₂Na.It is monoclinic and crystallizes in space group C2/c, Mr=1495.09, a=12.175(5), b=22.01(1), c=20.875(9)Å, β=99.04(4)°V=5575(5)Å³;Z=4;Dc=1.78g/cm³.Final R factor is 0.066.The result reveals that the[Mo₄S₄] cluster core and t-(dtp)-1 ligands are retained and only μ-bridged(dtp)^-1ligands are substituted by(C₆H₅CO₂)^-1 in the substitution reaction, thus producing the new title cluster compound, the structure of which contains two species of bidentate ligand.

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CRYSTAL STRUCTURE OF DI(α-HYDROXYISOBUTYRATE)DIAQUO NEODYMIUM NITRATE Nd(C₄H₇O₃)₂NO₃2H₂O

Cheng XU, Zhao Ai NI

中国化学快报. 1991, 2(07): 555-556.

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The crystal structure of di(α-hydroxyisobutyrate)diaquo neodymium nitrate Nd(C₄H₇O₃)₂NO₃2H₂O was determined by X-ray diffraction analysis.It belongs to monoclinic, space group C2/C, with cell dimensionsa=8.996(1), b=8.601(1), c=21.111(3)Å, β=92.38°, V=1632.OÅ³, Z=4, Dc=1.83g/cm³.Crystal structure has been refined by full-matrix least-square techniques giving a final R value of 0.036.The neodymium atom is coordinated to eight oxygen atoms.The nitrate group in complex is not bonded to neodymium, each two neodymium atoms are linked by bridging carboxyl group forming a chain polymeric molecule.

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CRYSTAL STRUCTURE OF FIVE-COORDINATE ZIRCONOCENE COMPLEX (MeCp)₂ZrC1(α-C₁₀H₇COO)

Zhi Qiang WANG, Shi Wei LU, He Fu GUO, Ning Hai HU

中国化学快报. 1991, 2(07): 557-560.

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(MeCp)₂ZrCl(α-C₁₀H₇COO) has five-coordinate bent zirconocene in which the α-naphthoyloxy is a bidentate ligand(Zr-O 2.317(2), 2.260(2)ÅZr-Cl 2.521(1)ÅZr-C 2.480-2.550ÅZr-cent-CH₃C₅H₄ 2.217, 2.23OA;Cl-Zr-O1 134.8(1)⁰;Cl-Zr-O2 78.6(1)^O;O1-Zr-O2 56.3(1)^O).

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THE STUDY OF COPOLYMERIZATION OF p-DIETHYNYLBENZENE WITH OTHER ACETYLENIC DERIVATIVES

Yin Kui LI, Zhao Hui CHEN

中国化学快报. 1991, 2(07): 561-564.

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The copotymerizations of p-diethynyibenzene(PDEB)with phenytacetylene(PHA), 4, 4'-diethynytbiphenyt(DEBP)or m-diethynylbenzene(MDEB)are studied in various mole ratios of monomers.The sotubitity parameter(σ_p), swellabitity(θ_p), Huggins parameter(X), density (d₄²⁵)and the average motecutar weights between crosstinks (M_c) of obtained copotymers are measured.The IR spectra of these copolymers are recorded.The mechanism about the polymerization of acetytenic derivatives initiated by(Ph₃P)₂PdCl₂ is discussed.

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PHOTOSENSITIVITY OF CERIC ION INITIATED METHYL ACRYLATE POLYMERIZATION

Jian Hua DONG, Jian Qing YANG, Kun Yuan QIU, Xin De FENG

中国化学快报. 1991, 2(07): 565-566.

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The polymerization of methyl acrylate was sensitive to UV light.Under UV light, the rate of polymerization is 8 times as high as the rate in dark.The overall activation energy was decreased by the UV light(313nm).A tentative explanation is given and the mechanism is discussed.

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SOAPLESS EMULSION COPOLYMERIZATION IN THE PRESENCE OF BARIUM SULFATE POWDER

Li CHEN

中国化学快报. 1991, 2(07): 567-568.

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To investigate soapless emulsion copolymerization in the presence of a solid phase, copolymerization experiments were carried out for the styrene-butyl acrylate-K₂S₂O₈-water system by using barium sulfate powder, which is assumed to be chemically inert.Reaction conditions were varied with respect to barium sulfate powder quantity, initiator concentration and temperature.These factors were investigated with respect to the effect on reaction rate and conversion, polymer particle number and diameter, and latex stability.

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THE STUDY ON THE KINETICS AND MECHANISM OF THE REACTIONS OF METAL IONS WITH PnAO

Bin SONG, Qi Yan ZHANG, Yun Ti CHEN, R. K. MURMANN

中国化学快报. 1991, 2(07): 569-570.

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The kinetics and the mechanism of the formation reactions of M(PnAO)²⁺(M=Ni, Co, Cu)were studied with UV Spectrophotometer and Stopped Flow Spectrophotometer and a three steps mechanism was suggested.

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A STUDY ON THE INTERACTION BETWEEN CH₃OH AND H₂CO MOLECULES IN TERMS OF THE PROPERTIES OF CHARGE DENSITY DISTRIBUTIONS^①

Wei Liang CAO, Jing Chang ZHANG, Xiao Yuan FU

中国化学快报. 1991, 2(07): 571-574.

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Two possible complexes formed by the interaction of CH₃OH and H₂CO, one hydrogen-bonded(Ⅰ) and one donor-acceptor complex(Ⅱ), have been reported in the previous paper⁽¹⁾.Based on the ab initio 6-31G basis set calculations, the properties of the charge density for the complexes have been analyzed using the theory of atoms in molecules^(2-5).The nature of the complex formation has been discussed in terms of the properties of the charge density distributions.

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COMPACT COIL OF LACQUER POLYSACCARIDE:FURTHER EVIDENCE

Xing Ping QIU, Li Na ZHANG, YU Min DU, Bao Gong QIAN, Zai Min LU

中国化学快报. 1991, 2(07): 575-576.

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The weight average molecular weights Mw, radii of gyration2>^1/2second virial coefficients A₂, and intrinsic viscosities in θ solvent [η]_θ of five fractionated samples of the chinese lacquer polysaccharide were measured by light scattering and viscosimetry.It is further evidenced that the polysaccharide in aqueous solution exists as a compact coil resulted from highly branched structure.

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THEORETICAL STUDIES ON THE THERMOLYSIS OF THIETANE

Guang Ju CHEN, Xiao Yuan FU, Ao Qing TANG

中国化学快报. 1991, 2(07): 577-578.

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The mechanism of the thermolysis of thietane to form ethylene and thioformaldehyde has been studied by using ab initio SCF MO method at STO-3G* and 3-21G* level.It has been found that there are two possible stepwise pathways.One is to break C-C bond firstly, while the other is to break C-S bond at first.The cleavage of C-S bond is pre-ferred over that of C-C bond.

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CATALYTIC PERFORMANCE OF ETHYLENE HYDROFORMYLATION OVER [H_XRu₃(CO)₉(CCO)]^2-X/SiO₂-Al₂O₃, SiO₂ AND MgO(X=0-2)CATALYSTS

Feng Shou XIAO, RuRen XU, Masaru ICHIKAWA, Duward F. SHRIVER, Xie Xian GUO

中国化学快报. 1991, 2(07): 579-580.

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The various surface species [H_XRu₃(CO)₉(CCO)]^2-X(X=0-2)prepared from impregnation of [PPN]₂[Ru₃(CO)₉(CCO)] on SiO₂-Al₂O₃, SiO₂ and MgO show quite different activities and selectivities for oxygenates and ethane in ethylene hydroformylation.

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CHARACTERIZATION OF COBALT SITES IN REDUCED Co-Mo/Al₂O₃ AND Ru-Co-Mo/Al₂O₃ CATALYSTS

Fend Shou XIAO, Qin XIN, Xie Xian GUO

中国化学快报. 1991, 2(07): 581-582.

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The two Co sites are well characterized in reduced Co-Mo/Al₂O₃ and Ru-Co-Mo/Al₂O₃ by new bands at 1895 and 1880 cm^-1 in the IR spectra due to NO adsorption.

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Formation of Methane and Ethylene in Methanol Conversion over HZSM-5 Catalyst

Bo Qing XU, Juan LIANG, Su Qin ZHAO, Guo Quan CHEN

中国化学快报. 1991, 2(07): 583-586.

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Primary formation of methane and secondary formation of ethylene in methanol conversion are evidenced by temperature-programmed-surface-reaction of adsorbed methanol on HZSM-5 catalyst.A reaction mechanism accounts for the observed results is described.

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SYNTHESIS AND CHARACTERIZATION OF RARE EARTH METAL COMPLEXES WITH PIPERONAL ISONICOTINOYL HYDRAZONE

Ming Xiong WAN, Han Qiu DEAN, Wei Da SHAN, Pei Zhi CHEN

中国化学快报. 1991, 2(07): 587-588.

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Complexes of La(Ⅲ), Nd(Ⅲ), Sm(Ⅲ), Eu(Ⅲ), Gd(Ⅲ), Dy(Ⅲ), Er(Ⅲ), Yb(Ⅲ)and Y(Ⅲ) with piperonal isonicotinoyl hydrazone(HPIN) have been synthesized in DMF and EtOH.The complexes have been characterized by elemental analysis, molar conductance, i.r., UV and ¹H n.m.r.spectra, magnetic measurements, X-ray powder diffraction and DTA.

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SPECTROSCOPIC PROPERTIES OF THE PHYCOBILINS AND THEIR DERIVATIVES

Ling Jiang CHENG, Li Jin JIANG

中国化学快报. 1991, 2(07): 589-592.

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The UV-VIS spectroscopic studies of phycoerythrobilin dimethyl ester, phycocyanobilin dimethyl ester and their derivatives indicate that shortening of the conjugative systems induces hypsochromic shifts in wavelength and increases in molar extinction coefficients in visible part;both zinc ion coordination and acetic acid treatment induce bathochromic effects for the phycobilins and their derivatives.

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THE INTRAMOLECULAR AROMATIC-RING STACKING INTERACTION OF MIXED LIGAND PALLADIUM(Ⅱ) COMPLEXES Ⅲ.STUDIES ON THE Pd²⁺-A-UTP^4- SYSTEMS BY ¹HNMR

Yu Qiu GONG, Hong Liang SUN

中国化学快报. 1991, 2(07): 593-594.

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The intramolecular aromatic-ring stacking interaction of mixedligand complex Pd(A)(UTP)^2- in the system pd²⁺-A-UTP^4- has been determined by ¹HNMR, where A=1, 10-phenanthroline(phen), 2, 2'-bipyridyl(bpy)and DL-tryptophan(trp^-);UTP^4-=uridine 5-triphosphate.The result indicates that it is the partial stacking between the uracil ring of UTP^4- and the heterocyclic ring of A that makes H(5), H(6) and H(1') in the UTP^4- shift upfield significantly.Accordingly, the order of aromaticring interaction in the mixedligand complex has been obtained as follows:Pd(phen)(UTP)^2- > Pd(bpy)(UTP)^2- > Pd(trp)(UTP)^3-.

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1991年, 第2卷, 第07期　刊出日期：1991-07-20

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1991年, 第2卷, 第07期 刊出日期：1991-07-20

1991年, 第2卷, 第07期　刊出日期：1991-07-20