中国化学快报

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STUDIES ON GLYCOSIDES XVII——STEREOSELECTIVE SYNTHESIS OF (2,6-DIMETIIOXY-4-ETHOXYCARBONYL) PHENYL 6-O-ACETYL-2,3,4-O-BENZYL-β-D-GLUCOPYRANOSIDE

Jian Min MAO, Jian ZHANG, Hong Ming CHEN, Meng Shen CAI

中国化学快报. 1994, 5(12): 1003-1004.

摘要 ( )

可视化

The key intermediate (7) to clemochinenoside-A (1),(2,6-dimethoxyl-4-ethoxylcarbonyl)phenyl 6-O-acetyl-2,3,4-O-benzyl-β-D-glucopyranoside has been stereo-selectively synthesized in high yield.

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SYNTHESIS OF 3-ARYL-1(2H, 4H) ACRIDONES AND THEIR DERIVATIVES

Rong YIN, Guang Fan HAN, Yu Tian LI, Jin Jun WANG, Gui Ji Jiang

中国化学快报. 1994, 5(12): 1005-1006.

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3-Aryl-1(2H,4H)acridones and the related acridine-fused pyridine,pyrimidines and quinolines were synthesized.The compounds synthesized have been not reported until now.The structures of all the compounds synthesized were characterized by elemental analysis,IR and ¹HNMR spectra.

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FACILE AND HIGHLY STEREOSELECTIVE SYNTHESIS OF (2Z)-α-PHENYLSELENO-α,β-UNSATURATED KETONES

Zhi Zhen HUANG, Xian HUANG, Yao Zeng HUANG

中国化学快报. 1994, 5(12): 1007-1008.

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α-Phenylseleno-α-acylmethylene triphenylarsoranes(3) were synthesized by reacting α-acylarsonium ylides(1) with phenylselenenyl iodide.The α-seleno arsonium ylides(3) have sufficient activity to carry out Wittig type reaction,affording the first method for the stereoselective synthesis of (2Z)-α-phenylseleno-α,β-unsaturated ketones(6).

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STUDIES ON THE PRENYLFLAVONOIDS PART XI:THE TOTAL SYNTHESIS OF (±)-AMORISIN AND (±)-SIGMOIDIN-B

Lian Yun ZHAO, Yu Lin LI

中国化学快报. 1994, 5(12): 1009-1012.

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Amorisin and Sigmoidin-B has been synthesized by demethylation of 3-methoxy-4-hydroxy-5-prenylbenzaldehyde followed by condensation of 3,4-dimethoxy methoxy-5-prenylbenzaldehyde with 2-hydroxy-4,6-dimethoxymethyoxy-3,5-diprenylacetopenone phenone and 2-hydroxy-4,6-dimethoxymethoxyaceto-phenone,cyclization and demethoxymethylation.

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LEWIS ACID MEDIATED RING F OPENING-ACETYLATION OF STEROIDAL SAPOGENIN

Wei Sheng TIAN, Hui Ping GUAN, Xin Fu PAN

中国化学快报. 1994, 5(12): 1013-1016.

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Treatment of steroidal sapogenin diosgenin 1 with Lewis acid ethereal trifluoroborane in acetic anhydride at room temperature afforded a new type of pseudosapogenin 23,26-diacetyl-△²²⁽²³⁾-pseudo-sapogenin 3 and its C-20 isomer 4 in 54% and 19% yield respectively.The possible mechanism was also suggested.

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THE FORMATION OF 1,2-BISDIPYRRINONE-ETHYLENES

Jin Shi MA, Qing Qi CHEN, Chang Qi WANG, Ling Jiang CHENG, Sheng JIN

中国化学快报. 1994, 5(12): 1017-1020.

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A new type of bile pigments,1,2-bisdipyrrinone-ethylenes (1).were obtained with promising yields(25,28,28.5%,for the respective samples)by bromine oxidation of dipyrrinones(2)in methylene chloride.

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PERFLUOROALKYLATION OF TYROSINE

Wei Yuan HUANG, Rui Qing LEE

中国化学快报. 1994, 5(12): 1021-1022.

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The intermediary perfluoroalkyl radical generated from the reaction of perfluoroalkyl iodide with sodium dithionite was shown to be reactive toward tyrosine esters,resulted in the formation of meta-substituted products which can be transformed into the corresponding amino acids after removal of the carboxyl protected groups of the esters.Thus,the rcaction provides a novcl method to introduce a perfluoroalkyl group into the aromatic ring of tyrosine in the meta-position.

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STUDIES ON THE SYNTHESIS AND DNA-BINDING ABILITY OF ZINC FINGER MOTIF

Xiao Yu HU, Rui WANG, Xiang Qun LI

中国化学快报. 1994, 5(12): 1023-1026.

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可视化

Transcription factor SP1 is a protein present in mammalian cells that binds to GC box promoter elements of Gene and selectively activates mRNA synthesis.The gene contains functional recognition sites.It contains three continuous zinc finger motifs,which are believed being metalloprotein structures that interact with DNA.We synthesized the second zinc finger fragment of SP1 (SP1-ZF2) and its mutant (SP1-ZF2/HT.E²⁰→H.R²³→T),we also synthesized the Cys-Cys loop (ZF6) and the His-His loop (ZF5) of SP1 and linked the two loops together using a β-turn structure to obtain a finger mimic analogue (ZF-15) by stepwise solid-phase technique.Atomic absorption studies show that SP1-ZF2 and SP1-ZF2/HT bind zinc equimolarly,but ZF-15 does not bind Zn anyway.The CD experiments demonstrate a significant change in secondary structure in the presence or absence of Zn to SP1-ZF2 and SP1-ZF2/HT,but there is no change about ZF-15.Gcl-retardation electrophoresis assays indicate that SP1-ZF2 binds to DNA sequence specifically in the presence of Zn,but SP1-ZF2/HT does not bind as SP1-ZF2 did.We observed that a single zinc finger like SP1-ZF2 is able to bind DNA sequence specifically.

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SYNTHESIS, COMPLEXATION PROPERTIES AND CRYSTAL STRUCTURE OF NEW DIOXOCYCLAM BEARING 8-METHYL QUINOLINE AS FUNCTIONAL PENDANT(S)

Dao Li AN, Xian lle BU, Xin Ying LIU, Yu LIU, Yun Ti CHEN

中国化学快报. 1994, 5(12): 1027-1030.

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Two new dioxo tetraamine ligands L₁ and L₂ hare been synthesized and characterized by ¹H NMR,IR,MS and elemental analysis,Their protonation constants and complex formation constants with Cu²⁺ have been determined by potentiometric titratioa.The X-ray crystal structure of L₁ has been determined.

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THE CRYSTAL STRUCTURE AND STEREOCHEMISTRY OF BENZOYL KETENE O,S ETHYLENE ACETAL

Shu Jia ZHANG, Ji Geng TANG, Qun LIU, Yan XING, Yong Hua LIN

中国化学快报. 1994, 5(12): 1031-1032.

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The crystal structure of the title compound 4,synthesized from benzoyl ketene dimethylthio acetal 3 and mercaptoethanol under basic condition,shows it has Z-configuration.This result supports that the formation of 4 is controlled by the stereoelectronic effects and 6 is the key intermediate.

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A NEW FLAVONE FRON EPIMEDIUM KOREANUM

Wen Kui LI, Pei Gen XIAO, Jing Qi PAN, Mu Jian LU, Ru Yi ZHANG

中国化学快报. 1994, 5(12): 1033-1034.

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可视化

A new flavone,epimedokoreanin D was isolated from the aerial parts of Epimedium koreanum.Its structure was determined by spectroscopic methods (UV,IR,MS,¹H NMR,¹³C NMR,DEPT) and chemical evidences.

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STRUCTURAL STUDIES OF A FROM THE POLLEN OF PAPAVER SOMNIFERUM

Ping MIAO, Song GAO, Sheng JIN

中国化学快报. 1994, 5(12): 1035-1036.

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A water soluble polysaccharide isolated from the pollen of Papaver somniferum has a main chain composed of 6-linked galactopyranosyl,2,3-and 2,4-linked rhamnopyrancsyl residues.It has an ordered structure which was investigated on the basis of KOH-induced absorption shifts and circular dichroism changes of polysaccharide and polysaccharide-Congo Red compiexes.

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DETERMINATION OF PROTEIN USING CATALYTIC COLORIMETRY OF SULFANILIC ACID BY COBALT(Ⅱ)

Yun Xiang CI, Xiao Da YANG, Xiao Ting TANG

中国化学快报. 1994, 5(12): 1037-1038.

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A new protein analysis method by the use of sulfanilic acid-hydrogen peroxide(H₂O₂)-Co²⁺ system was described.The method was based on the inhibition effect of protein on the catalytic activity of Co²⁺ for the coloration of sulfanilic acid.It took advantages of rather mild assay condition(pH 9.0),similar responses for albumin and globulin,and little interference.The assay could have a dynamic range of 0-1.00 mg/mL with a detection limit of about 0.01 mg/mL.

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A SENSITIVE PROTEIN ASSAY BY Co(Ⅱ)-BIURET METHOD

Yun Xiang CI, Xiao Ting TANG, Xiao Da YANG

中国化学快报. 1994, 5(12): 1039-1040.

摘要 ( )

可视化

A new and sensitive Co(Ⅱ)-biuret method for determination of protein has for the first time been established.In visible wavelength region,the Co(Ⅱ)-protein complexes had an absorption peak at 360 nm.-Under the present conditions,the assay had a linear range of 0-120 μg/ml of protein with a detection limit of about 2 μg/ml,and similar calibration curves were obtained for BSA.and BγG.Compared with Cu(Ⅱ)-biuret method,the present Co(Ⅱ)-biuret method,was more simple,sensitive,and tolerant of interferences from non-protein molecules.

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INVESTIGATION ON SIMPLE OSCILLOGRAPHIC VOLTAMMETRY WITH FEEDBACK VOLTAGE

Jian Bin ZHENG, Hong GAO

中国化学快报. 1994, 5(12): 1041-1042.

摘要 ( )

可视化

Simple oscillographic voltammetry with feedback voltage is presented in this paper.Experimental circuit and advantages of the method are given.

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GENOTOXICITY OF NICOTINE STUIED BY ACCELERATOR MASS SPECTROMETRY

Xin Song LI, Yuan Fang LIU, Jin Yuan SHI, Xiang Yun WANG, Ke Xin LIU, Zhi Yu GUO, Kun LI, Chia Erh CHEN, Si Xun YUAN

中国化学快报. 1994, 5(12): 1043-1044.

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可视化

DNA adduction with nicotine in mouse liver at environmental doses has been observed using ¹⁴C-label by accelerator mass spectrometry(AMS).An improved detection limit of DNA adducts of 1 adduct per 10¹¹ nucleotides has been given.It is primarily proposed that nicotine appears carcinogenic via its conversion to nitrosamines.

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STUDY ON COMPOSITION AND STABILITY CONSTANTS OF THE INCLUSION COMPOUNDS OF β-CYCLODEXTRIN WITH DIPHENYL AND ITS DERIVATIVES BY NMR

Le Xin SONG, Xiao Yuan CHEN, Qin Jing MENG, Xiao Zeng YOU

中国化学快报. 1994, 5(12): 1045-1046.

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可视化

The composition and stability constants of 2:1 inclusion compounds of β-cyclodextrin (β-CD) with guest molecules were obtained approximately by NMR method,for the first time,through changes of chemical shifts for H-3 of β-CD cavity.The guest molcculcs in the present work are diphenyl and its derivatives (p-hydroxydiphenyl;2,2'-dihydroxydiphenyl;4,4'-dihydroxydiphenyl).

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STUDY ON THE SECOND SPHERE COORDINATION COMPOUND

Le Xin SONG, Xiao Yuan CHEN, Qin Jing MENG, Xiao Zeng YOU

中国化学快报. 1994, 5(12): 1047-1048.

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One-to-one inclusion compound of (η⁵-cyclopentadien) tricarbonylmanganesc (MnCp(CO)₃, guest) with β-cyclodcxtrin (β-CD,host) was obtained in a crystalline state.The host-guest compound is thermally stable and do not liberate the guest on heating at 100℃ in vacuum.From the measurements of ¹H-NMR spectra and the model building with Corey Pauling Koltum (CPK) models, the most probable inclusion mode is proposed.

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NMR STUDY ON THE CONFORMATION CHANGE IN THE AGGREGATION PROCESSES OF 1,3-DI(α-NAPHTHYL)PROPANE AND DI(α-NAPHTHYLMETHYL)ETHER

Rui Qsing XIE, Zi Zhong LI, You Cheng LIU, Xue Gong LEI

中国化学快报. 1994, 5(12): 1049-1050.

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NMR study on the conformation change in the aggregation process of the titled compounds is reported in this letter.

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STUDIES OF FAR-INFRARED SPECTRA AND SOLID-SOLID PHASE TRANSITION IN [n-C_nH_2n+₁NH₃]₂CuX₄ LAYER COMPOUNDS WITH n=7-12,16

Ning GUO, Xing Jia GUO

中国化学快报. 1994, 5(12): 1051-1052.

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可视化

Far-infraraed spectra of the title compounds (abr.C_nCuX) have been studied.Empirical assignments of the main bands have been made.The solid-solid phase transition at T_p=38℃ in C_aCuCL compound has been investigated by the far-infrared spectra with variation of temperatures.It is found that the solid-solid phase transition of this compound was accompanied by the distortion disorder of the MCL₆^2- octahedra.

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INFRARED STUDIES OF CO/AI₂O3 CATALYSTS:CO and NO INTERACTION

Xin Sheng LI, Qin XIN

中国化学快报. 1994, 5(12): 1053-1054.

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可视化

When the Co/AI₂O₃ sample was heated in CO and NO mixture at above 473K,new bands at 2181 and 2253cm^-1 were observed,and presumably assigned to Co-NCO and Al₂O₃-NCO species,respectively.

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CRYSTAL STRUCTURE OF THE COPPER(Ⅱ) COMPLEX OF NEW MACROCYCLIC DIOXOTETRAAMINE LIGAND FUNCTIONALIZED WITH 8-METHYL QUINOLINE PENDANT

Xian He BU, Dao Li AN, Man Xue YUAN, Yun Ti CHEN

中国化学快报. 1994, 5(12): 1055-1056.

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The copper(Ⅱ) complex (1) of a new ligand 4-(quinolin-8-ylmethyl)-1,4,7,10-tetraazacyclotridecane-11,13-dione(L)has been synthesized and its crystal structure determined.It is of orthorhomic crystal system and Pcab space group with a=16.260(3),b=7.739(2),c=27.530(9)?,Mr=416.97,Z=8,Dx=1.595g/cm²,μ=12.876cm^-1,and F(000)=1736.The final R factor is 0.061 for 2594 observed reflections with I>3^σ(I).The Cu atom is five coordinated to form a distorted square pyramid geometry in which N(11)of the pendant is at apical site.

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SYNTHESIS OF TETRAMETHYLDISILANDIYL DICYCLOPENTADIENYL LANTHANIDE COMPLEXES AND STRUCTURE OF[Me₄Si₂(C₅H₄)₂Sm(μ-Cl)(THF)]₂

Fu Quan SONG, , Guo Liang LU, , Zhao Yu WANG, , Xiu Zhong ZHOU

中国化学快报. 1994, 5(12): 1057-1058.

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可视化

The reaction of Me₄Si₂(C₅H₄)₂Na₂ with LnCl₃ in THF leads to the formation of Me₄Si₂(C₅H₄)₂LnCl,(Ln:Nd(3),Sm(4),Gd(5),Y(6))or Me₄Si₂ (C₅H₄)₂Ln (C₅H₅)(THF)n(Ln:La(1) n=1,Pr(2) n=0);complex (4) was recrystallized in THF to form [Me₄Si₂(C₅H₄)₂Sm(μ-Cl)(THF)]₂ in space group P2₁/c with a=12.982(3),b=12.269(3),c=13.681(2) ?,β=96.79(2)° for Z=2,R=0.068.

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SYNTHESIS, STRUCTURE AND PROPERTIES OF THE COMPLEX OF COPPER CHLORIDE WITH A STABLE RADICAL

Zong Hui JIANG, Bai Wang SUN, Dai Zheng LIAO, Wei ZHANG, Geng Lin WANG, Xin Kan YAO, Hong Geng WANG

中国化学快报. 1994, 5(12): 1059-1062.

摘要 ( )

可视化

A novel complex formed by copper chloride and nitronyl nitroxide radical,NITphOMe [2-(4-methoxy-pheny)-4,4,5,5-tetramethyl-imidazoline-1-oxyl-3-oxide],was obtained.The complex has been charactrerized by elementary analysis,IR,UV-vis spectra and x-ray crystal structure analysis.

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SYNTHEIS, SITUCTURE AND CHARACTERIZATION OF BINUCLEAR Cu(Ⅱ) COMPLEX [Cu(C₆H₅COO)₂(C₅H₆N₂)]₂.(C₄H₄O)₂

Rui Na YANG, Dou Man JIN

中国化学快报. 1994, 5(12): 1063-1066.

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可视化

At room temperature,dibenzoyl peroxide undergoes oxidative addition on metallic copper powder and 2-aminopyridine in a mixed solvent(acetone and tetrahydrofuran),which affords the product as a binuclear Cu(Ⅱ) complex [Cu (C₆H₅COO)₂(C₅H₆N₂)]₂.(C₄H₈O)₂.The structure of the complex was characterized by elemental analyses,IR spectra,TG-DTA.The structure of the compound has been solved by direct method and Fourier synthesis,and refined by block-diagonal and full matrix least-squares method to a final R of 0.04329 for 3671 independent reflection of I>3σ(Ⅰ).The crystals are triclinic,C₄₆H₄₅N₄O₁₀Cu₂,Z=1,Mr=943.93,space group P-1,with cell parameters,a=10.806(1);b=11.169(3);c=11.729(2)?;α=71.99(2),β=89.38(1)°;γ=81.37(1);V=1330.1 ?⁸;Dc=1.172g.cm^-3;μ=8.5cm^-1.The copper(Ⅱ) ion is coordinated by four bridging bidentate benzoate and two 2-aminopyridine to form dimeric molecules.

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STUDY ON THE EXTRACTION OF BROMINE BY EMULSIFIED LIQUID MEMBRANE TECHNIQUE

Tong WANG

中国化学快报. 1994, 5(12): 1067-1070.

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可视化

The separation and enrichment of bromine from seawater by emulsion liquid membrane method were studied.The effect of separation process is also discussed and proper separation parameters are proposed.

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PREPARATION OF CdS NANO-PARTICLES IN MIXED SURFACTNT VESICLE SYSTEM

Guo Xi ZHAO, Wang Lin YU

中国化学快报. 1994, 5(12): 1071-1074.

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可视化

CdS particles were generated in the mixed sodium 10-undecenoate--decyltrimethylammonium bromide vesicle dispersions.Depending on the condition and method of preparation,CdS semiconductor absorption edges were found to range from 526 to 448 nm,corresponding to particle diameter between >5.0 and 2.7 nm.

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THE EFFECT OF ACID TREATMENT ON THE STABILITY OF POLYMORPHS IN BETA ZEOLITE

Jian Ping SHEN, Jun MA, Jun GUO, Da Zhen JINAG, En Ze MIN

中国化学快报. 1994, 5(12): 1075-1078.

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The stability of beta zeolite in acid solution and the effect of acid treatment on the polymorphs in beta zeolite were studied.This zeolite is easily dealuminated by HCl treatment but its framework highly resistent to acidity.In β zeolite,polymorph A is less stable than polymorph B.The chirality of β zeolite can be modified by the method of acid treatment.

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1994年, 第5卷, 第12期　刊出日期：1994-12-20

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1994年, 第5卷, 第12期 刊出日期：1994-12-20

1994年, 第5卷, 第12期　刊出日期：1994-12-20