中国化学快报

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Studies on the Reaction of Benzopyran-4-one with Hydroxylamine Hydrochloride

Zheng YAN, Wen Long HUANG, Wei Yi HUA, Si Xun PENG

中国化学快报. 1997, 8(02): 95-96.

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It is reported that 6-methyl-flavanone oxime would rearrange to isoxazoline in the presence of trifluroacetic acid and the rearrangement would not take place in anhydrous ethanol with catalytic amount of pyridine.However,6-nitro-benzopyran-4-one when treated with hydroxylamine hydrochloride,gave oxime and its isomeric isoxazoline through rearrangement under acid or alkali condition.

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Studies on Chiral Thiophosphoric Acids and Their Derivatives 15.The Asymmetric Cyclizations of L-prolinol with (Thio) phosphoro(-no) dichlorides

Chu Chi TANG, You Ming WANG, Zheng Jie HE

中国化学快报. 1997, 8(02): 97-98.

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The cyclizations of L-(+)-prolinol 1 derived from L-proline with (thio) phosphoro(-no) dichlorides 2 give 1,2,3-azaphosphaoxabicyclo[3.3.0]octanes 3 consisting of unequal amounts of diastereoisomers,eight pairs of which have been successfully separated by silica gel column chromatography or recrystallization.

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Construction of the Oxetane Ring from 5α-Acyloxy-Δ⁴⁽²⁰⁾-taxoids

Rui Wu LIU, Ji Yu GUO, Xiao Tian LiANG

中国化学快报. 1997, 8(02): 99-100.

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An oxetane ring can be constructed from 5α-acyloxy-△⁴⁽²⁰⁾-taxoids with osmylation as the first step in the usual manner.The innovation reported here is the use of an intramolecularly available acyl group for the protection of 20-OH by an unexpected 5-to 20-migration under slightly basic conditions.

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Total Synthesis of (±) Kadsurenin M

Ming Yi WANG, An Xin Wu, Xin Fu PAN, Xiao Jiang HAO, Chang Xiang CHEN

中国化学快报. 1997, 8(02): 101-102.

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Kadsurenin M (7s,8s-3,4,3'-trimethoxy-7'-oxo-nor-8',9'-7.O.4'-8,5'-neolignan) (1),a benzofuranoid neolignan isolated from the aerial part of Piper Kadsura (Choisy) Ohwi,was synthesized in 6 steps from vanillin via a key intermediate 3,4-dimethoxycinnamyl (2'-methoxy-4'-formyl) phenyl ether (7).The overall yield is 15%.

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Total Synthesis of (+) Villosol

Ping XIE, Shu Feng CHEN, Xiao Tian LIANG

中国化学快报. 1997, 8(02): 103-106.

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The total synthesis of (+)villosol was accomplished by using the readily available (-)2 as starting material.

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Proton-Template Synthesis of a П-Conjugated Macrocycle and Structure of its Ni₂ (Ⅱ)-Complex

Yun Qi TIAN, Jian TONG

中国化学快报. 1997, 8(02): 107-110.

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A metal-free Robson-type macrocycle was synthesized for first time by proton-templation and from that the metal complexes were prepared.By X-ray study the structure of Ni(I)-complex was characterized.

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Chemo-Enzymic Synthesis of a Four-Chiral-Center Portion of A-23187 (Calcimycin)

Jian Wen Fang, Zu Yi LI

中国化学快报. 1997, 8(02): 111-113.

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A four-chiral-center portion of A-23187 was synthesized from a chiral synthon which was obtained from lipase-catalyzed resolution.

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Synthesis of New Ointment-like Poly (ortho esters)

Zheng Rong LU, Jia Hui YU, Ren Xi ZHUO

中国化学快报. 1997, 8(02): 114-116.

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可视化

Ointment-like poly(ortho esters) were synthesized from the reaction of 3,9-bis (methylene)-2,4,8,10-tetraoxaspiro[5.5] undecane with PEG-400,N,N-bis(2-hydroxyethyl)-n-hexadecylamine and N,N-bis(2-hydroxyethyl) palmitamide respectively.The influence of the catalyst on the intrinsic viscosity of polymers was also studied.

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Trimethylammonium Chlorochromate Adsorbed on Alumina:a New Reagent for the Oxidation of Alcohols to the Corresponding carbonyl Compounds

Gui Sheng ZANG, Qi Zeng SHI, Mi Feng CHEN, Kun CAI

中国化学快报. 1997, 8(02): 117-120.

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A new reagent.trimethylammonium chlorochromate adsorbed on alumina.suitable for the oxidation of hydroxy compounds to the corresponding carbonyl compounds is described

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Studies on the Reaction Mechanism of CO₂-Reforming of Methane over Co/γ-Al₂O₃ Catalyst

Yong LU, Chang Chun YU, Jin Zhen XUE, Yu LIU, Xue Jia DING, Shi Kong SHEN

中国化学快报. 1997, 8(02): 121-124.

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TPPR and XPS characterizations were combined to study the reaction mechanism of CO₂-reforming of methane to syngas over Co/γ-Al₂O₃ catalysts.CH₄ shows a tendency to form surface carbons by deep dissociation at high temperatures.CO₂ dissociation reaction also occurs at >673K.It is believed that carbide carbons are active species to generate CO by reacting with O atoms dissociated from CO₂.In the reaction,Co⁽⁰⁾ particles are responsible for dissociating CH₄ to form active C.abstracting an O atom from CO₂ molecule,and transferring O atom to C to form CO.

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Five New Glycosides, Ligurobustosides E, F, I, J and K from Ligustrum Robustum

Jun TIAN, Hong Jie ZHANG, Han Dong SUN, Lu Tai PAN, Pin YAO, De Yuan CHEN

中国化学快报. 1997, 8(02): 125-128.

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Five new monoterpenoid glycosides named ligurobustosides E(1),F(2),I(3),J (4) and K (5) were isolated from the leaves of Ligustrum robustum.Their structures were established by spectroscopic and chemical methods.

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Five New Compounds from Clerodendrum Indicum

Jun TIAN, Qin Shi ZHAO, Hong Jie ZHANG, Zhong Wen LIN, Han Dong SUN

中国化学快报. 1997, 8(02): 129-132.

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From the aerial parts of Clerodendrum indicum,five new compounds,cleroindicins B-F (1-5) were isolated and their structures identified by spectral method.

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Studies on Chemical Constituents of Belamcanda Chinensis (L.)DC.(Ⅱ)

Li Xin ZHOU, Mao LIN

中国化学快报. 1997, 8(02): 133-134.

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Nine compounds were isolated from the acetone soluble fraction of ethanolic extract of the roots of Belamcanda chinensis (L.)DC.The structure of new compound I,named shegansu A,has been established as irigenin-5-0-(6"-O-vanillin acid)-β-D-glucoside(I) by the use of spectroscopic evidence (UV,IR,FAB-MS,¹HNMR,¹³CNMR,¹H-¹³CNMR and NOE difference spectrum) and chemical methods.The well known compounds were identified as isorhapotigenin (Ⅲ),resveratrol(Ⅳ),p-hydroxy benzoic acid (Ⅴ),iridin (Ⅵ),tectoridin (Ⅶ),tectorigenin (Ⅷ) and daucosterol (Ⅸ).Ⅲ-Ⅸ were isolated from the plant for the first time.

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Lactariolide, a New 14-Membered-Ring Compound from Lactarius Subvellereus

Jing ZHANG, Xiao Zhang FENG

中国化学快报. 1997, 8(02): 135-136.

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Lactariolide (Ⅰ),a new 14-membered-ring lactone was isolated from the fruit bodies of Lactarius subvellereus (Russulaceae),and its structure was elucidated as (R)-13-hydroxy-trans-9,11-octadecadienoic acid lactone by means of physical and spectral data.

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Hemsleyasine, a New Norditerpenoid Alkaloid from the Roots of Aconitum Hemsleyanum Var.Circinatum

Qing Yan Xu, Feng Peng Wang, Timothy Chit-ming, Chun Tao Che

中国化学快报. 1997, 8(02): 137-140.

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A new norditerpenoid alkaloid,hemsleyasine 1,has been isolated from the roots of Aconitum hemsleyanum var.circinatum W.T.Wang and its structure was established by spectral methods (¹H-and ¹³C-NMR,¹H COSY,COLOC and nOes).

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Studies on the Relationship between the Helical Structure and Optical Activity of Some Chiral Cyclic Esters Ⅱ

Ai Hua NIE, Xiu Lin YE, Qi Yi XING

中国化学快报. 1997, 8(02): 141-144.

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A method for the analysis of the relationship between the helical structure and optical activity was proposed by the study of the conformations and X-ray diffraction structures of some cyclic esters prepared by esterification of L-(-)-2,3-O-methylidene threitol and L-(+)-2,3-O-isopropylidene threitol with alkanedioyl dichlorides and o-,m-,and p-phthaloyl dichlorides.

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A Study on the Inclusion of α-Cyclodextrin with Mono-and 1,4-Disubstituted Benzenes by Neural Networks

Qing Xiang GUO, Shi Dong CHU, Yong Min WANG, Zhong Xiao PAN, Mao Sen ZHANG, You Cheng LIU

中国化学快报. 1997, 8(02): 145-148.

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可视化

The association constant (K_a) values were calculated by the function-strengthening neural networks (FNN) for the inclusion complexation of α-CD with mono-and 1,4-disubstituted benzenes.The lnK_a predicted by FNN from R_m,π and σ constants of substituents are in great agreement with the experimental data.

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Kinetic Studies on Reactions of Monocyclic Oxyphosphoranes with Ethylene Glycol

Nan Jing ZHANG, Xin CHEN, Yu Fen ZHAO

中国化学快报. 1997, 8(02): 149-152.

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The reaction of monocyclic oxyphosphorane compounds 1a,1b,1c with ethylene glycol in pyridine was studied by ³¹P NMR.The results show that compound 1a with an unsaturated five-membered ring reacts faster than compound 1b with a saturated ring attached by two trans p-nitro phenyl groups,which in turn reacts greatly faster than the cis-compound 1c.To interpret the mechanism,a hexacoordinate intermediate whose five-membered ring occupied the e-,e- position was proposed.

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Calculations of Chemical Reaction Dynamics for D+H₂(j_i, ν_i=0)→DH(j_f, ν_f=0)+H

Li Qin SI

中国化学快报. 1997, 8(02): 153-156.

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The constant Centrifugal potential approximation is Corrected so as to apply to the reactions of rotational excited reactants for D+H₂(j_i,ν_i=0)→DH(j_f,ν_f=0)+H.Our results show that the contributions from j_i≠0 and Ω_i terms are not negligible.

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Synthesis, Relaxivity and Biodistribution of Novel Magnetic Resonance Imaging (MRI) Contrast Agents:Polylysine (Gd-DTPA/DOTA) with Pendent Galactose Moieties as Hepatocyte-targeting Groups

Ren Xi ZHUO, Yan Jun FU, Jun LIAO

中国化学快报. 1997, 8(02): 157-160.

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DTPA or DOTA ligand was introduced into the pendent amino groups of polylysine (DP 268) by mono-mixed anhydride of DTPA or DOTA,and then translated with Gd-EDTA.The resultant polymer chelates were further reacted with 6-O-bromoacetyl-D-galactose to give liver-specific contrast agents for magnetic resonance imaging.These new polymer conjugates were characterized by FT-IR,ICP-AES,UV-Vis spectrophotometry and elemental analysis.Their in vitro spin-lattice relaxivity and body distribution in mice were investigated.

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Thin-Layer Chromatographic Separation of Amino Acid Enantiomers using Ligand Exchange

Qing Ying DENG, Zhang ZHANG, Jing Yu SU

中国化学快报. 1997, 8(02): 161-164.

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Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers.The chromatographic selectivity and the effects of plate different preparation methods,sample molecular structure and solvent compositions on resolution performance were also discussed.

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Two Side Chain β-CD Polysiloxanes Used as New Stationary Phase for Chiral Separation by HRGC

Han Bang ZHANG, Yun LING, Ruo Nong FU, Yu Xiu WEN

中国化学快报. 1997, 8(02): 165-166.

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Two new stationary phases:(Ⅰ)[bikis(2,6-di-O-pentyl-3-O-hex-6-enyl)-pentakis(2.6-di-O-pentyl-3-O-methyl)-β-CD-polysiloxane] and (Ⅱ)[heptkis(2,6-di-O-methyl-3-O-hex-6-enyl)-β-CD-polysiloxane] were synthesized and successfully used for GC separation of chiral isomers.They possess high column efficiency and exhibit fine chiral separation ability.

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Electrolytic Sampling from Pure Copper and Common Brasses Ⅰ:Calculation of the Mass Dissolved from the Samples according to Faraday's Law

Jin ZHANG, Jian Nan YANG

中国化学快报. 1997, 8(02): 167-170.

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In a procedure for electrolytic dissolving pure copper and common brasses,the approximate electrochemical mole mass(k) of the sample was determined in accordance with the brand of the sample,a suitable electrolyte was selected to make the current efficiency equal to 100%,and then the dissolved mass of samples was calculated according to Faraday's law (m=kIt).Three representative samples were sampled by the electrolytic dissolution method and the calculated dissolved amounts were equal to the values by weighing the anode.The experimental results of zinc and copper in the anode liquor are in agreement with certified values.

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Spectroelectrochemical Studies on Poly-o-phenylenediamine 1. In-situ Resonance Raman Spectroscopy

Ling Ling WU, Jin LUO, Zhong Hua LIN

中国化学快报. 1997, 8(02): 171-174.

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The structure of poly-o-phenylenediamine in the redox process has been studied using in-situ resonance Raman spectroscopy,in-situ UV-Vis subtractive reflectance spectroscopy and cyclic voltammetry.The results show that the structure of PoPD is dominated by a ladder polymer with phenazine rings,and at least three structures of PoPD are formed in the redox process.The three kinds of PoPD have different resonance enhancement effect,and the electronic structure of PoPD molecule is influenced obviously by protonation.The results also show that the most stable state of PoPD is its semi-oxidized state.

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Effects on the Surface Passive Film of Carbon Anode on Cell Behavior

Shu Hua MA, Ji LI, Xia Bin JING, Fo Song WANG

中国化学快报. 1997, 8(02): 175-176.

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The properties of the films formed in the electrolyte of PC/DME LiClO₄ on two kinds of carbon materials were examined by cathodic polarization measurements.The result suggested that the films on both carbon electrodes have different morphology which resulted in the different cell performance of the two carbon anodes.

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Lutetium:a Special Lanthanide Prefers Dimer in Fullerene Cages

Chun Yan HAO, Xing Hua GUO, Zi Yang LIU, Da Yong SUN, Shu Ying LIU

中国化学快报. 1997, 8(02): 177-180.

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可视化

Endohedral dilutetium fullerenes,Lu₂@C_2n (2n=76~112),have been extracted from the soot prepared by arc-burning method for the first time and different from other lanthanide encapsulated fullerenes,there is no signal corresponding to Lu@C₈₂ even in mass spectrum of the high-temperature,high-pressure extract.

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Study on the Interaction of Rare Earth with 3, 5, 3'-Triiodothyronine

Feng GAO, Shu Yun WANG, Shu Lan MENG, Yan Min LIU, Chun Ji NIU, Jia Zuan NI

中国化学快报. 1997, 8(02): 181-182.

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The stability constants for rare earth complexes with 3,5,3'-triiodothyronine were determined at 37℃ and an ionic strength of 0.15 mole/L NaCl.The lanthanide induced shifts were measured for ¹H nuclei of 3,5,3'-triiodothyronine.The coordination of rare earth with 3,5,3'-triiodothyronine was discussed.

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Preparation of Fe₃O₄/PS Magnetic Particles by Dispersion Polymerization

Xiao Bin DING, Hua Zhong SUN, Guo Xiang WAN, Ying Yan JIANG

中国化学快报. 1997, 8(02): 183-184.

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可视化

Fe₃O₄/PS magnetic particles with core/shell structure has been prepared in the presence of Fe₃O₄ magnetic fluid in ethanol/water mixture.Magnetic particles with diameter size range from 5.54 to 187.32 μm were obtained by different reaction conditions.Some parameters such as ethanol,PEG and monomer which affect particle size diameter and size distribution are discussed briefly in this paper.

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Preparation of GaN Powder of Nanometer Scale by MOCVD Using DEGA as Precursor

Yu Ming ZHAO, Ke Yan ZHOU, Yun Cheng YUAN

中国化学快报. 1997, 8(02): 185-188.

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可视化

GaN powder of nanometer scale was prepared by metal organic chemical vapor deposition using diethylgallium azide as precursor.The resulting powder was characterized by XRD and TEM.It has been found that the particle size of the powder obtabed is affected by the deposition temperature,and the fine crystals formed m temperature range 500~650℃ were hexagonal.

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1997年, 第8卷, 第02期　刊出日期：1997-02-20

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1997年, 第8卷, 第02期 刊出日期：1997-02-20

1997年, 第8卷, 第02期　刊出日期：1997-02-20