中国化学快报

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SYNTHESES OF TWO NEW UNICARBON-CHAIN BIS (BENZO-15-CROWN-5) COMPOUNDS

Li LIN, Jin Liang GUO, Yong LI

中国化学快报. 1991, 2(10): 751-752.

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Carbonyl bis (4'-benzo-15-erown-5) has been synthesized by heating the mixture of benzo-15-crown-5 and 4'-earboxybenzo-15-crawn-5 in polyphosphoric aeid (PPA), and bis (4'-benzo-15-crown-5) carbinol is obtained by reducing carbonyl bis (4'-benzo-15-crown-5) with sodium borahydride. A use ful method is provided to synthesize various types of symmetrical and unsymmetrical bis (crown ether)s.

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MICHAEL REACTION OF CHLOROESTERS IN A TWO-PHASE SOLID-LIQUID SYSTEM

Chao Guo YAN, Qiang Zhi KONG, Wen Xing LU, Ji Tao WU

中国化学快报. 1991, 2(10): 753-754.

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The Michael addition of α-chloroesters to α,β-unsaturated systems was catalyzed by traalkylammonium salt in a two-phase solid-liquid system, and some polysubstitnted evclopropanes were facilely synthesized.

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A NEW CONVENIENT METHOD FOR THE SYNTHESIS OF PERFLUOROALKYL 2H-PYRROLE

Wei Yuan HUANG, Wu Ping MA

中国化学快报. 1991, 2(10): 755-756.

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The reaction between 2,5-Dimethylpyrrole (1) and R_FI (2) (R_F:a, Cl (CF₂) ₄; b, Cl (CF₂) ₆; c, Cl (CF₂) ₈; d, n-C₆F₁₃; e, n-C₈F₁₇) in the presence of Na₂S₂O₄-NaHCO₃ in acetonitrile resulted in the formation of 2-perfluoroalkyl-2,5-dimethyl-2H-pyrrole (3) as a major product in good yield.

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STUDIES ON SYNTHESIS OF SUGAR NUCLEOTIDES

Tian Wei MA, Ji Mei MIN, Li He ZHANG

中国化学快报. 1991, 2(10): 757-760.

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Glucosyl phosphotriester of adenosine and glucosyl thiophosphotriester of adenosine were synthesized by phosphite-triester methodology.

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THE REARRANGEMENT OF 1,7β-DIMETHYL-7α-HYDROXY-8aα-CARBOXYMETHYL-9β-CARBOMETHOXY-4bα, 5, 6, 7, 8, 8a-HEXAttYDROFLUORENE LACTONE INDUCED BY DIBAL-H

Hun Ping HU, Xin WANG, Xin Fu PAN

中国化学快报. 1991, 2(10): 761-752.

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1,7β-Dimethyl-7α-hydroxy-8aα-carboxymethyl-9β-carbomethoxy-4bα, 5, 6, 7, 8, 8α-hexahydrofluorene lactone (2) is converted to 8, 12-epoxyallogibberic acid methyl ester (4) by the action of diisobutyl aluminum hydride (DIBAL-H) with a novel rearrangement reaction.

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A NEW AND EFFICIENT SYNTHESIS OF 3-IODO DERIVATIVES OF FLAVONES, THIOFLAVONES AND THIOCHROMONES

Fang Jie ZHANG, Yu Lin LI

中国化学快报. 1991, 2(10): 763-764.

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The title compounds are prepared in good yields by iodination of the corresponding flavones, thioflavones and thiochromones respectively using I₂-CAN (ceric ammonium nitrate) system. The compounds thus prepared are potentially useful precursors for the synthesis of C-3 linked binuclear compounds.

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SECOND ORDER NONLINEAR OPTICAL PROPERTIES OF DICYANOPYRAZINES

Cheng YE, Zhi Ming FENG, Yan Jun CHEN, Jia Fu WANG, Hai Ou DONG

中国化学快报. 1991, 2(10): 765-768.

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Second order nonlinear optical active 2,3-dichloro-5,6-dicyanopyrazine (DCDCP) and its monoamine-substituted derivatives had been synthesized. Their facile synthesis, high melt point, high incidence af substantial SHG activity and increased transparency inthe blue and near infrared make this class compounds appealling for further investigation.

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(Z)-ETHYL 3-BROMO-4,4,4-TRIFLUORO-2-BUTENOATE AS A NOVEL CF₃-CONTAINING BUILDING BLOCK:Its Preparation and Pd-Catalysed Reaction with Alkynes and Organozinc Reagents

Wei Yuan HUANG, Long LÜ

中国化学快报. 1991, 2(10): 769-772.

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A novel CF₃-containing building block, (Z)-ethyl 3-bromo-4,4,4-trifluoro-2-butenoate, was easily prepared from CF₃CBr₃, the former reacted with alkynes Or organozinc reagents in the presence of Pd complexes to afford useful CF₃-containing intermediates in good yield.

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SOLID-PHASE SYNTHESIS OF 4,5-DISUBSTITUTED 1,2,3-TRIAZOLES

Chen Xi LI, Wen Qiang HUANG, Yu LU, Bing Lin HE

中国化学快报. 1991, 2(10): 773-774.

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4-Aryl-5-ethoxycarbonyl-1-H-1,2,3-triazoles have been prepared by treatment of ethyl polystyrylsulfonylacetate with substituted benzaldehydes and then sodium azide.

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STUDIES ON THE CHEMICAL CONSTITUENTS OF CLAUSENA LANSIUM (LOUR.) SKEELS Ⅳ THE STRUCTURAL ELUCIDATION OF SECO-AND SECODEMETHYL-CLAUSENAMIDE

Ming He YANG, Liang HUANG

中国化学快报. 1991, 2(10): 775-776.

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The spectral data and chemical properties of two new amides isolated from Clausena lansium led to the assignment of acyclic structures of C-6 and C-7. The absolute configurations of the two chiral carbons in C-6 were determined by degradation to be 3S4R.

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STUDIES ON CYCLOPENT-2-ENONE:(Ⅲ) THE STUDY ON DECONJUGATION OF CYCLOPENT-2-ENONE ALDOL ADDUCTS

Xiao An Zhang, M. M. Campbell, D. W. Brown

中国化学快报. 1991, 2(10): 777-780.

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Deconjugation of cyclopent-2-enone aldols were attempted under various conditions, and the desired deconjugated product was achieved via dianion approach. Various results obtained in this study are explained by structure and transition state analysis.

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SYNTHESIS AND STRUCTURE OF [4Ni (SALEN)·GGH] CLO₄·EtOH·H₂O (GG=Glycylglyciae)

Zi Ming SUN, Yan WANG, Kai Bei YU

中国化学快报. 1991, 2(10): 781-782.

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The complex of [4Ni (salen)·GGH] CLO₄·EtOH·H₂O has been synthesized and studied by X-ray single crystal analysis. The results show that there are both intra-unit hydrogen bonds in the [4Ni (salen)·GGH]⁺ and inter-unit hydrogen bonds between the two [4Ni (salen)·GGH]⁺. Ni (salen) in the unit are still centrosymmetric dimers with planar structure. Imide N(10)-H(10) in the [GGH]⁺ bonds with one phenolic oxygen 0(7) of Ni (salen) dimer in the same unit. Two H atoms of amino group N (9)-H[H (A), H (C)] in the glycylglycine perchlorate interact with phenolic oxygen[0 (3), 0 (5)] of [4Ni (salen)·GGH]+ through two strong hydrogen bonds respectively.

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PSEUDO π IONIZATION POTENTIALS OF H-(CH₂) _n-X

Yi WANG, Li LI

中国化学快报. 1991, 2(10): 783-784.

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By means of the energy level formula E (p)=α+2βcos (pπ/(n+t+1)). the pseudo π ionization potentials of H-(CH₂)_n-X (X=H, F, Cl, Br, I, OH, and SH) are identified by optimizing linear regression analysis, from which α=13.54±0.50eV and β=1.75±0.13eV are obtained.

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A NEW NOR-SESQUITERPENOID FROM THE SOFT CORAL PARALEMNaLIA THYRSOIDS

Jing Yu SU, Yong Li ZHONG, Jian Qing WU, Long Mei ZENG

中国化学快报. 1991, 2(10): 785-786.

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A rare nor-sesquiterpenoid with a γ-spirolactone, pathyiactone A (1), was isolated from the soft coral Paralemnalia thysoides. The structure and absolute stereochemistry of 1 was established by spectral analysis, especially 2D NMR and difference NOE studies, and CD method.

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FUZITINE A NEW APORPHINE ALKALOID FROM FU ZI (ACONITUM CARMICHEALI DEBX)

Hai sheng CKEN, Gong Yu HAN, Ming Zhu LIU, Hua Qing LIANG

中国化学快报. 1991, 2(10): 787-788.

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A new aporphine alkaloid, named fuzitine, was isolated from the tuber of Aconitum carmicheali Debx, and its chemical structure was established'on the basis of spectral analysis and chemical reaction.

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STUDY AND APPLICATION OF SPECTROPHOTOMETRIC DETERMINATION OF MICRO AMOUNTS OF BISMUTH WITH MESO-TETRAKIS-(4-N-TRIMETHYL AMMONIUMPHENYL) PORPHINE

Mei FANG, Shou Kun HU

中国化学快报. 1991, 2(10): 789-792.

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A new highly sensitive spectrophotometric method has been developed for the determination of micro amounts of bismuth (Ⅲ), based on the formation of Bi (Ⅲ)-meso-tetrakis-(4-N-trimethylammonium phenyl) porphine [T (4TMAP) P] complex. In the presence of Cd (Ⅱ), Bi (Ⅲ) reacts almost instantaneously with T (4TMAP) P in a 0. 6 mol/l NaAc-HAC buffer (PH5.8) at room temperature. The composition of the complex is T (4TMAP) P:Bi=1:1. The absorbance complex obeys Beer's law over the Bi (Ⅲ) concentration range 0.1-1.4 μg/ml. The linear relative coefficient γ is 0.9998. The apparent molar absorptivity was 1.75×10⁵ 1.mol^-1. cm^-1 at 463nm. The relative standard deviation of the method is 1.50% for Bi (Ⅲ) 7ug/10ml (10 determinations). The interference of foreign ions has been examined. This simple and rapid method can be applied to the assay of Bi (Ⅲ) in some tablets directly.

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AN EASY-TO-MAKE OZONE GENERATOR FOR THE IMMOBILIZATION OF STATIONARY PHASES IN GC CAPILLARY COLUMNS

Bing Jiu XU, Shan Nian DONG

中国化学快报. 1991, 2(10): 793-796.

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An easy-to-make ozone generator which can be made with readily available materials is proposed. Concentration of the ozone prepared with this generator could reach that of ozone in equilibrium with oxygen. Cured with the ozone thus prepared, GC capillary columns with immobilized SE-54 phase and excellent chromatographic performance were successfully prepared.

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MASS SPECTROMETRY SYNTⅡESIS OF PHENYL COBALT TETRAPHENYI. PORPHYRIN

Xiang GAO, Zi Yang LIU, Wei Ping JIA, Shu Ying LIU

中国化学快报. 1991, 2(10): 797-800.

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It has been found that phenyl cobalt tetraphenylporphyrin (C₆H₅Cotpp) was formed when cobalt tetraphenylporphyrin (Cotpp) and benzene were introduced into the ion source of mass spectrometer, the mass spectra of Cotpp and C₆H₅Cotpp are discussed.

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CRYSTAL STRUCTURE OF SEVEN-COORDINATE TRIPODAL MANGANESE (Ⅱ) COMPLEX

Shao Hua GOU, Zheng XU, Xiao Zeng YOU

中国化学快报. 1991, 2(10): 801-802.

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MnC₂₄H₂₇F₁₂N₇O₃P₂·C₂H₅OH, Mr-852, orthogonal, space group P21 3, a=15.220 (2)Å;Z=4; V=3525 (1)Å³; F (000)=1732; Dc=1.61g/cm³; μ=5.52cm^-1 (Mo Kα=0.71073Å). Manganese (Ⅱ) atom is seven-coordinated, with the coordination polyhedron of a monocapped antitrigonal prism.

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SYNTHESIS AND STRUCTURE OF TWO-ELECTRON HETEROPOLY BLUE K₂H₄SiMoⅤ₂Mo (Ⅵ) ₁₀O₄₀·12H₂O WITH α-KEGGIN STRUCTURE

En Bo WANG, Lan Cui ZHANG, Zuo Ping WANG

中国化学快报. 1991, 2(10): 803-804.

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The single crystal of two-electron heteropoly blue with Si as the heteroatom and α-Keggin structure K₂H₄SiMoⅤ₂Mo (Ⅵ) ₁₀O₄₀·12H₂O was obtained by electrolytic reduction. It crystallizes in a triclinic system with space group P1, Mr=2117.73, a=13.702 (4), b=14.107 (3), c=14.184 (2)Å; α=119.27 (1), β=93.14 (2),;γ=110. 3 (2)°, V=2154.29Å³, Z=2, F (000)=1999, μ=36.39cm^-1, Dc=3.26 g/cm³. Final R factor is 0.0515. Mo (Ⅴ) is situated in two different edge-shared Mo₃O₁₃ groups. The heteropoly blue was characterized by IR, UV, polarography, X-ray photoelectron spectra and ESR. All the results show that the structure of the heteropoly anion with Keggin structure remains unchanged basically in the process of reduction.

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RAP ID FIUORIMETRIC DETERMINATION OF TRYP TOP HAN BY THE R (?) ACTION WITH CERIUM (Ⅳ)

Nian Qin JIE, Jing He YANG, Xue Feng LIU

中国化学快报. 1991, 2(10): 805-808.

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A flmorimetric method for determination of typtophan was proposed. This method is very simple, rapid in determination of tryptophan in aqueous medium. The percentage of recovery was satisfactory.

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APPLICATION OF MONTE-CARLO SIMULATED ANNEALING ON CONFORMATIONAL ANALYSIS

Qiao Lin DENG, Yu Zhen HAN, Lu Hua LAI, Xiao Jie XU, You Qi TANG

中国化学快报. 1991, 2(10): 809-812.

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Mothod (SA) was applied to the conformational analysis of flexible molecules such as peptides. The programs SAMM and SAPEP have been developed, using MM2 force field for organic molecules and ECEPP/2 force field for peptides respectively.nte-Carlo simulated annealing me

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Electrostatically Stabilized Aggregate (ESAg). Ⅰ. Evidence Derived from the Coaggregating Behavior of an Anionic Kinetic Probe (P16^-) with Surfactants

Xi Kui JLANG, Guo Zhen JI, Jian She WANG

中国化学快报. 1991, 2(10): 813-816.

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A newly proposed ESAg concept is verified by the coaggregation behavior of an anionic kinetic probe (P16^-) with various surfactants.

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SYNTHESIS OF A NOVEL AMPHIPHILE, 4-[4-(4-DECYLOXYPHENYLAZO) NAPHTHYLOXY] BUTYL TRIMETHYLAMMONIUM BROMIDE, AND ITS SELF-ASSEMBLING BEHAVIOR IN DILUTE AQUEOUS SOLUTION

Guo Wen LI, Xue Wen HU, Hong DING, Ying Qiu LIANG

中国化学快报. 1991, 2(10): 817-820.

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A novel amphiphile of 4-[4-(4-decyloxyphenylazo) naphthyloxy] butyl trimethylammonium bromide has been synthesized. It can form the stable bilayer in dilute aqueous solution.

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INDUCTION-POLYMERIZATION OF PREPARING POLYMERS OF REGULAR STRUCTURE

Hsiao Lin CHANG, You An Map, Yi Men CHENG

中国化学快报. 1991, 2(10): 821-822.

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Induction-Polymerization is a novel method for preparing polymers of regular structure. In the presence of a special macromolecular compound, monomer molecules are aggregeted regularly around one or more growth points and polymerized to polymer of regular structure. Regularity of structure of the polyacrylamide prepared by this means has been verified with electron diffractograms, DSC curve and IR spectrum of the polymer.

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EFFECTS OF BAICALEIN, WOGONIN, BAICALIN AND Na₂MoO₄ ON N-NITROSATION REACTION

Yu FANG, Dao Dao HU, Zi Li ZHAO, Yun Chao MA, Zuo Min SUN

中国化学快报. 1991, 2(10): 823-826.

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The in vitro effects of baicalein,wogonin,baicalin and Na₂MoO₄ on N-nitrosation reaction have been studied. The N-nitrosation reaction has been determined by the amount of dimethylnitrosamine (DMN) and diethylnitrosamine (DEN) produced using the UV-photclysis spectrophotometric and pyrolysis gas chromatography test. Baicalein,wogonin and Na₂MoO₄ showed varing extents of inhibition of the formation of DMN and DEN. Baicalin promoted the formation of DMN and DEN under the condition of simulating gastric Juices. It is also found that E. coli showed a remarkable promoting effect on the formation of DMN and DEN,but this promoting effect could be blocked to some extent by baicalein,wogonin,baicalin and Na₂MoO₄. Besides, Na₂MoO₄ and wogonin have shown synergic effect on the blocking of N-nitrosation reaction.

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Production of Superoxide Ion with Carbon Gas-Diffusion-Electrode And Reaction of Superoxide Ion with Aromatic Halide

Shu Fang WANG, Chu Bao HUANG, Dong ZHANG

中国化学快报. 1991, 2(10): 827-828.

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Superoxide ion O₂^- is prepared in aprotic media by carbon gas-diffusion-electrode for the first time. The experimental results indicate that this electrode is superior to carbon plane-electrode in the reaction of O2^- with p-bromonitrobenzene. When the gas-diffussion-electrode is used, the yield of the product nitrophenol increases by 20%, and the selectivity of the reaction is nearly doubled as compared with the plane-electrode.

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1991年, 第2卷, 第10期　刊出日期：1991-10-20

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1991年, 第2卷, 第10期 刊出日期：1991-10-20

1991年, 第2卷, 第10期　刊出日期：1991-10-20