1998 Volume 9 Issue 3

α-Oxoketene Cyclic S,S-cetals Chemistry-Substitution Reaction of α,α'-Dicinnamoyl Ketene Cyclic S,S-Acetals with Ethylenediamine
Mei Xin ZHAO , Qun LIU , Fu Shun LIANG , Jing Fu LIU , Bao Zhong ZHAO , Lian Zhong LI
1998, 9(3): 231-232
[Abstract](194) [FullText HTML] [PDF 69KB](0)
α, α'-Dicinnamoyl ketene cyclic S, S-acetals 4 were reacted with ethylenediamine to afford α, α'-dicinnamoyl ketene cyclic N, N-acetals 5. This process provides a new method for the synthesis of 5 in high yield under mild conditions.
Diels-Alder Reactions of 3-Carboethoxy-and 3-Carbonitrile-2-Cyclohexen-1-one
Wen Qian YANG , Shi Zhi CHEN , Liang HUANG
1998, 9(3): 233-234
[Abstract](178) [FullText HTML] [PDF 93KB](0)
Aluminum chloride induced Diels-Alder reactions of 3-carboethoxy-and 3-carbonitrile-2-cyclohexen-1-one with cyclopentadiene, isoprene and (E)-piperylene were described. The stereochemistry of the adducts were confirmed by 2D-NMR spectroscopy and isomerization reactions.
Study of Intramolecular Cyclization of N-styryl-oxo-cinnamides (Ⅱ)
Nian Chun MA , Ke Mei WU , Liang HUANG
1998, 9(3): 235-236
[Abstract](181) [FullText HTML] [PDF 81KB](0)
The preparations and intramolecular cyclizations of amides 5, (N-methyl-N-(2-trans-2-phenylethenyl)-3-phenyl-2, 3-cis-oxiranecarboxamide) and 8, (N-methyl-N-(2-cis-2-phenylethenyl)-3-pheny 1-2, 3-cis-oxiranecarboxamide) were reported.
Novel Photoinduced Electron Transfer Reaction of N-methylphenothiazine in Carbon Tetrachloride
Xia GUO , Li YANG , Long Min WU , You Cheng LIU , Zhong Li LIU
1998, 9(3): 237-240
[Abstract](188) [FullText HTML] [PDF 148KB](0)
U. V. irradiation of N-methylphenothiazine 1 in carbon tetrachloride produced 3-(phenothiazin-N-yl-carbonyl)-N-methylphenothiazine 2 together with the radical cation salt 1+ CCl4- and methyl chloride, presumably via a photo induced electron transfer mechanism.
A Mild and Practical Procedure for Tetrahydropyranylation of Alcohols and Phenols Catalysed by Anhydrous Ferrous Sulfate
Tong Shuang LI , Zhan Hui ZHANG , Tong Shou JIN , Yu Lin LI
1998, 9(3): 241-244
[Abstract](186) [FullText HTML] [PDF 168KB](0)
An easy preparation of tetrahydropyranyl (THP) ethers of alcohols and phenols with 3, 4-dihydro-2H-pyran (DHP) in refluxing dichloromethane has been carried out in good to excellent yields under catalysis of anhydrous ferrous sulfate.
Design,Synthesis and Characterization of a Novel Schiff Base Bis (iminoantipyrine) and Its Modified Electrode
Jin Gang Liu , Fu Xin Xie , Sheng Yi Zhang , Yu Peng Tian , Shi Sheng Ni
1998, 9(3): 245-248
[Abstract](184) [FullText HTML] [PDF 173KB](0)
A novel Schiff base, N, N-bis[2-(2-iminoantipyrinephenoxy)ethyl]-p-toluenesulfonamide (BIAET), was synthesized and characterized, and a carbon paste electrode modified with BIAET was prepared and employed for quantitation of lead. The linear range, precision, limit of detection and interference have been investigated.
Synthesis of Oxa-Steroidal-Estrogen Analogues
Yong ZOU , Ling Ling WENG , Hu ZHENG
1998, 9(3): 249-250
[Abstract](190) [FullText HTML] [PDF 88KB](0)
The total synthesis of (±)-6-oxa-13β-ethyl-3-methoxy-8α-gona-1.3.5(10)-trien-17-one and (±)-6-oxa-13β-ethyl-2-methoxy-8α-gona-1.3.5(10)-trien-17-one was described.
An Efficient Synthesis of Heterocyclic Substituted Ureidoalkylphosphonates
Zai Guo LI , Run Qui HUANG , Hui Ying LI
1998, 9(3): 251-253
[Abstract](198) [FullText HTML] [PDF 106KB](0)
A convenient synthesis of various heterocyclic substituted ureidoalkylphosphonic acid diphenyl esters 3 is reported in this paper. a-Aminoalkylphosphonic acid diphenyl esters 1 reacted with triphosgene, and then treated with heterocyclic amines gave 3. Small amount of symmetric urylenediphosphonate 4 are isolated as side products.
Synthesis and Characterization of Poly (Aryl Ether Ketone) from Bis-1,4-(4-Chlorobenzoyl) Benzene
Yan Jun LIU , Xi Gao JIAN
1998, 9(3): 255-256
[Abstract](193) [FullText HTML] [PDF 76KB](0)
A new poly (aryl ether ketone) was successfully synthesized by nucleophilic substitution of bis-1, 4-(4-chlorobenzoyl) benzene (BCBB) by 1, 2-dihydro-4-(4-hydroxy phenyl) (2H)-phthalazin-1-one (DHPZ) in appropriate condition. The polymer was characterized by FT-IR, 1H-NMR, DSC and TGA etc.
Synthesis and Characterization of Poly (Ether Sulfone Ketone) Containing the Phthalazinone Moiety
Yan Jun LIU , Sheng Jun LIU , Xi Gao JIAN
1998, 9(3): 257-258
[Abstract](186) [FullText HTML] [PDF 78KB](0)
A novel poly (ether sulfone ketone) containing the phthalazinone moiety was prepared by the reaction of 4-)4-hydroxyphenyl) (2H) phthalazin-l-one with activated dichloro-monomers. The polymer was characterized by FT-IR, 1H-NMR, DSC, TGA and X-ray diffraction.
A New Method for the Synthesis of C/D Ring Synthon of Vitamin D
Ling Jie GAO , Tian Zeng ZHAO , Guang Dian HAN
1998, 9(3): 259-260
[Abstract](190) [FullText HTML] [PDF 92KB](0)
A C/D ring synthon of vitamin D is readily obtained from cholesteryl acetate via oxidation, elimination of acetoxy group and Norrish type Ⅱ photochemical reaction.
Chemical Studies on Decahydroacenaphthylene Compounds-Studies on the Synthesis of Hainanolide-Construction of Tricyclic Intermediate
Zheng Qi YANG , Shi Zhi CHEN , Liang HUANG
1998, 9(3): 261-262
[Abstract](187) [FullText HTML] [PDF 66KB](0)
The tricyclic compound is constructed via intramolecular Diels-Alder reaction. It might serve as the important intermediate for the total synthesis of hainanolide. The isolation and structures of three by-products were also described.
Preparation of Dendrimers from Macromolecular Cores and Papain Immobilization
Li Jian LIU , Shao Hua SHI , Ren Xi ZHUO , Zheng Rong LU
1998, 9(3): 263-264
[Abstract](184) [FullText HTML] [PDF 114KB](0)
Using amino-poly(ethylene glycol) and amino-propyl silica gel as initiator cores, two dendrimers were prepared by a two-step procedure. The progress of dendrimers during each step was monitored by infrared spectroscopy and elemental analysis. Papain was crosslinked to the solid dendrimer with silica gel core by glutaraldehyde, and the enzymatic activity of the immobilized papain kept almost unchanged after repeated usage for fifteen times.
Characteristic Studies of Arylated β-Cyclodextrins in Host-Guest Complexation with Small Molecules
Ai You HAO , Lin Hui TONG , Tian lin YANG , Ji Mao LIN
1998, 9(3): 265-268
[Abstract](189) [FullText HTML] [PDF 153KB](0)
The aryl moiety which was bonded as a functional group on the primary alcohol side of β-CD or the secondary alcohol side of β-CD or the secondary alcohol side of β-CD with an ethylenediamino chain could show remarkable different molecular recognition abilities in the complexation with small molecular guests such as alkanes, cycloketones etc.
Supramolecular Metal Complex with Ferrocene-conjugated Macrocyclic Triaza Crown Ether as Ligand and Its Electrochemical Property
Ye Gao YIN , Kung Kai CHEUNG , Wing Tak WONG
1998, 9(3): 269-272
[Abstract](191) [FullText HTML] [PDF 135KB](0)
A tetranuclear complex[CO(Ⅲ)2(L)2(AcO)2(OH)](AcO)(2I)4H2O (L=N-ferrocenyl-methyl-1, 4, 7-triaza-cyclononane) was prepared from ligand L HI and its crystal structure was determined. The crystal exists in P21/a space group and its cell parameters are α=14.285(3)Å, b=19.888(3)Å, c=19.133(3)Å; β=109.12(2)°; V=5135.8Å3; Z=4. Electrochemical investigation reveals that the oxidation potential of ferrocenyl group in 1 has a 0.11V-positive-shift from that of the ferrocenyl group in L. HI.
A Special Property of DNA——as an Electrocatalyst
DaiWen PANG , Qi LU , Min ZHANG , Shen HU , Zong Li WANG , Jie Ke CHENG
1998, 9(3): 273-276
[Abstract](194) [FullText HTML] [PDF 171KB](0)
A new special property of DNA was found. It can remarkably catalyze the electrooxidation of catecholamine neurotransmitters. The electrocatalytic activity of DNA towards catecholamine neurotransmitters can be attributed to the interaction between DNA and the neurotransmitters.
The Colour Reaction of Mercury with 1-(6-Ethoxyl-2-benzothiazolyl)-3-(4-Nitrophenyl)-Triazene and its Application
Chuan Ming JIN , Ming Hua YANG , Chu Ru GONG , Zhong Qiu HU
1998, 9(3): 277-279
[Abstract](182) [FullText HTML] [PDF 112KB](0)
A new triazene reagent 1-(6-ethoxyl-2-benzothiazolyl)-3-(4-nitrophenyl)-triazene (EtOBTNPT) has been synthesized. The colour reaction of EtOBTNPT with Hg(Ⅱ) has been studied. At pH=10.1-10.7, in the presence of Triton X-100, the reagent with Hg(Ⅱ) forms an orange-yellow complex with high sensitivity. The molar absorptivity is 2.38×105L·mol-1·cm-1. Beer's law is obeyed for Hg(Ⅱ) in the range of 0-7μg/25ml.
Electrochemical Reduction of Zearalenone
Zhi Qin WANG , Li XU , Wen Juan ZHOU , Cheng Ming ZHOU , Rong Sen YE , Ting Fang ZHANG , Wu Chang ZHAN
1998, 9(3): 277-230
[Abstract](170) [FullText HTML] [PDF 149KB](0)
Electrochemical reduction of zearalenone 1 and its derivatives was described. The ratio of a-and b-zearalanol 2 obtained by electrochemical reduction reached 8:1, much higher tan that obtained from catalytic hydrogenation. In addition to of the normal reduction products a rearranged product 5 was isolated. The reduction was supposed to be a electrocatalytical reaction.
HPLC Determination of Amino Acids by Pre-Column Fluorescence Derivatization with Carbazole-9-yl-Acetyl Chloride
Jin Mao YOU , Xing Jun FAN , Qing Yu OU , Qing Cun ZHU
1998, 9(3): 281-285
[Abstract](190) [FullText HTML] [PDF 202KB](0)
A sensitive HPLC method for the detection of amino acids with pre-column fluorescence derivatization with carbazole-9-yl-acetyl chloride has been developed. This method, in conjunction with a multi-gradient program, offers baseline resolution of the common CRAC-amino acids from a linear acetonitrile gradient. Separation of amino acid derivatives was obtained on a reversed-phase C18 column. Derivatization and chromatographic conditions were optimized. Amino acid derivatives were eluted in 40 min with good reproducibility. The relative standard deviations (n=6) at an analytical concentration of 100 pmol are <4%. The methods described are also suitable for the analysis of amino acids in different biological samples.
Selective Determination of Epinephrine by Using an Improved Modification of the Trihydroxyindole Method
Jing He YANG , Chang Lun TONG , Gut Ling ZHANG , Xia WU , Cun Guo Lin , Jing Tian HU
1998, 9(3): 287-289
[Abstract](176) [FullText HTML] [PDF 140KB](0)
A simple and selective method for the determination of epinephrine is put forward, which is an improved modification of the trihydroxyindole method. Experiment indicated that in borax buffer (pH=8.7) and with mercaptoethanol as the reducing reagent, dopa and dopamine did not form fluorescence products, so it is possible to determine epinephrine selectively.
High Order Harmonic A.C Oscillographic Chronopotentiometry
Jian Bin ZHENG , Ye Wei FU , Hong GAO
1998, 9(3): 291-294
[Abstract](188) [FullText HTML] [PDF 146KB](0)
Applying Fourier transform technique to deduction of background and noise on dE/dt-t curve, a new electrochemical method, high order harmonic oscillographic chronopotentiometry, is proposed in this paper.
A New Model for Correlating the Solubility of Solids in Supercritical CO2 and Study on Some Systems (Ⅱ):Correlation and Prediction
Ming Hong ZHONG , Bu Xing HAN , Jie KE , Zhi Min LIU , Hai Ke YAN , Ding Yu PENG
1998, 9(3): 295-298
[Abstract](183) [FullText HTML] [PDF 152KB](0)
Abstract The solubilities of a number of solid solutes in supercritical CO2 have been correlated using the model proposed in previous paper. The numbers of CO2 in each CO2-solute cluster and the local density of the CO2 in the clusters are predicted using the model. The results calculated agree fairly well with the experimental data.
Phase Transition Temperature of HPT (2,3,6,7,10,11-hexa-n-pentyloxytriphenylene) from Molecule Dynamic Simulation
Jun LUO , Tao WANG , Su Sheng TAN , En Le ZHOU
1998, 9(3): 299-303
[Abstract](178) [FullText HTML] [PDF 186KB](0)
Molecule dynamics simulation was used on HPT(2, 3, 6, 7, 10, 11-hexa-n-pentyloxy-triphenylene), which is a discotic liquid crystal. From analyzing the energy and displacement varying with the temperature, the phase transition temperature of PM6MPP can be predicted. The deviations of Tg, Tm and Ti due to the MD time scale are small enough that it should be possibly used to predict the material properties especially when more powerful computers are available.
The Electrochemical Behavior of PPV/PEO Blend
Chun He YANG , Jun Rong ZHENG , Yong Fang LI
1998, 9(3): 305-306
[Abstract](176) [FullText HTML] [PDF 90KB](0)
The electrochemical behavior of PPV/PEO blend with different dopants was investigated by cyclic voltammetry. The p-doping process is electrochemically quasi-reversible while the n-doping is irreversible. The band gap of the blend obtained by the cyclic voltammetry is 2.45 eV, which is the same with that of pure PPV.
A Gold Electrode QCM Study on the Self-Assembling Process of Thioglycollic Acid in Aqueous Solution
Qing Ji XIE , You Yu ZHANG , Da Zhong SHEN
1998, 9(3): 307-310
[Abstract](180) [FullText HTML] [PDF 139KB](0)
In this letter, the self-assembling process of thioglycollic acid on gold in aqueous solutions was studied by QCM technique. Frequency information suggests bilayer or multilayer adsorbate formation in 0.5 mol/L KCl solution but only monolayer one in 0.5 mol/L KOH solution. This phenomenon is explained by hydrogen bond effect.
Fabrication and Fluorescence Study of Sensitizing Dye/TiO2 Films
Hai Ning CUI , Li Ying WANG , Dong Met WANG , Gut Fen SUN , Shi Quan XI
1998, 9(3): 311-314
[Abstract](194) [FullText HTML] [PDF 134KB](0)
Fluorescence spectra of the sensitizing dye/TiO2 bilayer films were studied. Charge-transfer complexes were formed in the above bilayer.
Study of (TPP) H2 Vapor Deposited Film on Iron
Chuan Wei YAN , Li Ping GUO , Guang Ling SONG , Xiang Qin LIN , Chu Nan CAO , Hai Chao LIN
1998, 9(3): 315-318
[Abstract](176) [FullText HTML] [PDF 140KB](0)
The film by tetraphenyIporphyrin((TPP)H2) vapor deposition on iron was investigated by means of XPS, SEM and visible spectroscopy. N(1s) binding energy characteristic of (TPP)H2 was gained directly from the deposited samples. N(1s) binding energy of the surface was greatly changed after the deposited sample was washed with solvent. It is indicated that the deposited film is composed of an outer-layer of physically adsorbed (TPP)H2, and an inner-layer of chemically modified (TPP)H2.
Molecular Weight Distribution of Polyethylene Determined by high Temperature GPC
Pei Jun JI , Jian XU , Jin Shen WU , Mei Ling YE , Liang He SHI
1998, 9(3): 319-320
[Abstract](192) [FullText HTML] [PDF 79KB](0)
Molecular weight of polyethylene (PE) and its distribution were determined by PL-GPC210 at high temperature, 160℃ or 170℃. The thermostability of PE at high temperature was discussed and its real molecular weight can be obtained.
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