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中文
Table of Content
24 May 1990, Volume 11 Issue 5
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Articles
Studies on Some μ
3
-Oxo-bridged Trinuclear Manganese (Ⅲ)Schif f Base Complexes
Chen Ke, Chen Banglin
1990, 11(5): 443-448.
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Seven recently synthesized *3-oxo-bridged trinuclear Manganese(Ⅲ ) schiff base complexes-Mn
3
O(bzaea)
2
(C
2
H
3
O
2
)
3
, Mn
3
O(bzaea)
2
(C
2
H
3
O
2
)
2
(NCS), Mn
3
O(bzaea)
3
ClO
4
· 2H
2
O, Mn
3
O · (bzaea)
2
(C
2
H
3
O
2
)
2
Br, Mn
3
O(bzaea)
3
I · 2H
2
O, Mn
3
O(bzaea)
2
(C
2
H
3
O
2
)
2
NO
3
and Mn
3
O(bzaea)
2
(C
2
H
3
O
2
)
2
BPh
4
· 3H
2
O, where bzaea
2
-is the dianion of tridentate schiff base 2- (β-hydroxyethyl-imine)-4-phenyl-butanone(4), were studied by using the elemental analysis, electronic conductivity, magnetic susceptibity, thermal analysis, electronic and infrared spectra etc. The possible configurations of the complexes are suggested.
Synthesis and Structure Investigation of Borate Molecular Sieves
Wang Jianhua, Feng Shouhua, Xu Ruren
1990, 11(5): 449-453.
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Two novel microporous alumino-borates were synthesized from Na
2
O-CaO(MgO)-Al
2
O
3
-R
2
O
3
-R-H
2
O systems. X-Ray diffraction analysis(XRD), IRspectra and X-Ray photo-electron spec-troscopy analyses (XPS) show that the alumino-borates have novel framework structures. They exhibit charateristic adsoption properties like that of zeolite after the desorption of free water and other molecules within their structures. It is also shown that the micropore size of the alumino-borates are between 5～6Å.
Syntheses and Structures of Substituted Derivatives of Fe
3
(CO)
9
(μ
3
-S)
2
with P(SR)Cl
2
和P(SR′)
3
Suo Quanling, Liu Shutang, Hu Xiang, Liu Qiwang
1990, 11(5): 454-457.
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Six new mono- and three di-substituted derivatives of Fe
3
(CO)
9
(μ
3
-S)
2
with P(SR)Cl
2
and P(SR')
3
were synthesized. They have the formulas; Fe
3
(CO)
8
(μ
3
-S)
2
L [L = P (SC
6
H
5
)Cl
2
, P(SC
2
H
5
)Cl
2
, P(SC
3
H
7
)Cl
2
, P(SC
2
H
5
)
3
, P(SC
6
H
13
)
3
, P(SC
3
H
7
)
3
] and Fe
3
(CO)
7
(μ
3
-S)
2
L
2
[L = P(SC
6
H
5
)Cl
2
, P(SC
2
H
5
)
3
, P(SC
6
H
5
)
3
], respectively. The nine new compounds were characterized by elemental analysis and IR,
1
H NMR.MS spectra and the structure for Fe
3
(CO)
8
(μ-S)
2
[P(SC
6
H
5
]Cl
2
] was determined by means of four cycle diffractome-ter.
Syntheses and Characterizations of Benzylcyclopentadienyl Lanthanoid Dichloride
Zhang Bin, Wang Yuling, Bao Xiaohua, Chen Wenqi
1990, 11(5): 458-461.
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This paper reports the syntheses and characterizations of benzylcyclopentadienyl lanthanoid dichloride tetrahydrofuranate complexes. The complexes C
6
H
5
CH
2
C
5
H
4
LnCl
2
·
n
THF(C
6
H
5
CH
2
C
5
H
4
= Benzylcyclopentadienyl; Ln = Nd, Sm, Gd; n = 1, 2) were characterized by elementary analysis, thermal analysis, IR, MS, and
1
H NMR. The benzylcyclopentadiene is also characterized by the same method. The crystal structure of the intermediate C
5
H
6
CH
2
C
5
H
4
Na · THF was determined by X-ray diffraction analysis.
Studies on Adsorptive Voltammetry Behaviour of Molybdenum ( Ⅵ )-Mandelic Acid System
Xu Hongding, Liu Zaixin, Zhang Zhan'en, Zhang Lijun
1990, 11(5): 462-466.
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In this paper, a study of the adsorption voltammetry behaviour of Mo(Ⅵ)-mandelic acid (HL) is made systematically. The complex H
2
MoO
4
L
2
2-
can be adsorbed on the HMDE. The conditional constant of complex formation, 5. 7×10
9
, maximum amount of adsorption, 8×10
-7
mol/m
2
, and coefficient of adsorption, 1. 7 × 10
4
m
3
/mol, were determined in the medium of 2. 5 × 10
-3
mol/L H
2
SO
4
. A procedure for determining Mo by utilizing the adsorptive stripping current of the ad-sorptable complex is developed. The limit of detection is 5× 10
-10
mol/L Mo and the linear relationship between the current and concentration of Mo(Ⅵ) is in the range 1× 10
-9
～8× 10
-8
mol/L.
A New Method for Determination of the Kinetic Parameter of Reversible Reaction
Xu Liang, Gu Ztucheng
1990, 11(5): 467-470.
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A new method for determination of the reaction rate constant in the reversible pseudo first-order reaction was proposed. By this method, the rate constant of ligand exchange reaction between arsenzao Ⅲ coordinating with rare earth and CyDTA was determined. The principle of selecting kinetic data, which were used to calculate the reaction rate constant, was discussed in detail. The kinetic parameters have been applied to the differential kinetic analysis of binary mixture of rare earth with a satisfactory result.
Synthesis of Chloropropylpolysiloxanes alid Application to Gas Chromatographic Stationary Phases
Deng Shumei, Huang Mubin, Zhao Zhongxi, Yan Changtai
1990, 11(5): 471-475.
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The novel chloropropylpolysiloxanes were synthesized and used for gas chromatographic stationary phase. This new, moderately polar stationary phases exhibit higher-thermal stability (300～325℃) and can be used to separate non-polar and moderately polar compounds——n-alkanes, alkyl-benzenes, halogenated alkanes, esters and ketones. The McReynolds constants of these stationary phases are apparently higher than that of QV-17 and very similar to that of QF-1. The thermal stability and separation power of the alternating condensation polymers are better than that of the random copolymers. The stationary phase with 50% phenyl content could be crosslinked by 8% dicumyl peroxide. The vinyl group attached to the main chain may facilitate the crosslinking.
Application of Several Phosphorous Agents to the Preparation of Some Derivatives of 2-(4,5-Dihydro-4-Isopropyl-4-Methyl-5-Oxo-1H-Imidazoline-2-yl)-Benzoic Acid
Chen Ruyu, Liu Lijian
1990, 11(5): 476-480.
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This paper is about the application of several phosphorous agents to the synthesis of somederivatives of 2-(4,5-dihydro-4-isopropyl-4-methyl-5-oxo-1H-imidazoline-2-yl)-benzoic acid( I ) .Ireacted with O,O-diethyl phosphorochloridothioic ester to give out a mixture of 1 : 1 of 2-oxo-3-isopropyl-3-methyl-3H-imidazoine[2,1-a]-1-oxo-isoindole and its isomer. But when I was stirredwith hexaalkyl phosphorous triamide in THF N,N-dialkyl amide of I was isolated.
Synthesis and Characterization of Iron-Sulfur and Cobalt-Carbon Mixed Cluster Complexes μ-[(CO)
6
Co
2
PhC
2
S](μ-RS)Fe
2
(CO)
6
Song Licheng, Mbiyangandu Kadiata, Wang Jitao
1990, 11(5): 481-484.
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It was shown that the single Fe-Scluster core complexes of (μ-PhC≡CS) (μ-RS)-Fe
2
(CO)
6
1 could undergo a complexation reaction with Co
2
(CO)
8
in Et
2
O at room temperature, giving the Fe-Sand Co-C double cluster core complexes of μ-[(CO)
6
Co
2
PhC
2
S] (μ-RS)Fe
2
(CO)
6
2. Besides the structures of complexes 2 were characterized, the bond: type between Rand bridging sulfur atom and the influence of steric hindrance on the complexation reaction were also discussed.
Molecular Orbital Studies of n→π
*
Transitions of Formic Acid Monomer and Dimer Proton Transfer
Feng Jikang, Wang Qiming, Gao Zhiming, Li Jun, Li Zhiru
1990, 11(5): 485-490.
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The guound state, the lowest singlet and triplet n→π
*
states of the monomer and dimer of formic acid are studied with the MINDO/3 and INDO/S methods. The potential energy curves for the concerted transfer of two bridging protons are studied for all of the states. We explain the blue shift of the n→π
*
absorption band by the dimer with respect to the monomer successfully, and get the structure and energy of transition state.
The Study on Catalytic Properties of Perovskite Oxides of Iron
Ji Yushu, Wei Quan, Guo Benheng, Jian Bo, Uu Xiaoxun
1990, 11(5): 491-495.
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Ascries of La
1-x
A'
x
FeO
3
(A'=Ca, Sr, Ba; 0≤x≤1) was prepared. CO oxidation activity was studied when La was substituted partly by Ca, Sr, Ba and the crystal structure was measured by XRD. The adsorption properties were studied by XPS and TPD. It was found that the alkaline earth element substituted complex oxides (except that containing>0. 5 Ca and 1. 0 Ba) are of the perovskite type. Based on the obtained results it can be concluded that the adsorbed oxygen ions are responsible for the oxidation of CO. In addition, we tried to do some explanation for the activity of the mentioned reaction.
Studies on the Catalysts of Silicotungstic Acid in the Oxidative Dehydrogenation of Ethylbenzene
Wu Tonghao, Li Xia, Yang Hongmao, Wang Guojia, Jiang Yuzi
1990, 11(5): 496-500.
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We studied the catalytic behaviour of silicotungstic acid and its salt in the oxidative dehydrogenation of ethylbenzene to styrene. The carbonaceous material formed on the surface was considered to be the active sites for the oxidative dehydrogenation of ethylbenzene; the yield of styrene increases with the increase of C/H value of carbonaceous material; the specific surface of supports has a remarkable effect on the activation of catalysts. Benzole acid was discovered in the products and the oxidation of the carbonaceous material is the major source of CO
x
.
IRMPD Mechanism Study of Heterocyclic Compounds
An Xinyue, Guo Yongyou, Gu Yueshu, Liu Chuanpu, Hou Zhenglin, Yin Yongjia
1990, 11(5): 501-505.
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The infrared multiphoton dissociation (IRMPD) of 1,4-dioxane, pyrrolidine and thiophene were studied with TEA CO
2
laser. The mechanism involving breakage of carbon and heteroatom bonds were explored. The dependence of dissociation yield on laser energy was obtained. The laser dissociation threshold energy for dioxane, pyrrolidine and thiophene are 0. 85, 1.0 and 1. 5 J/cm
2
respectively.
Studies on the Phase Equilibrium of Oil/Water Interface of the Surfactant Solutions
Mao Qingcheng, Wu Shusen
1990, 11(5): 506-510.
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Based on Butler's equation and the relationship of phase equilibrium, this article suggests a scries of generalized equations for calculating phase equilibrium among the bulk phases and the interface phase. By using the equations proposed in this paper, the interfacfal mole fractions and the inter-facial adsorption amounts of the surfactant solutions can be calculated, and the calculation for several practical systems was carried out and the results obtained are satisfactory.Based on the experimental phenomena and calculated results, a physical model for the interface phase is suggested, the interaction among the surface active substances in the interface phase is also discussed and a lot of useful information are applied to the researches of emulsion, microemulsion etc.
Studies on Chelate Resins (ⅩⅢ) —— Syntheses and Adsorption Properties of New Chelating Resins with a Polythioether Backbone Bearing Pyridylamino Groups
Dong Shihua, Liu Fang, Hu Yunhua
1990, 11(5): 511-515.
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Three new chelating resins (PTAP- Ⅰ, PTAP- Ⅱ and PTAP- Ⅲ ) with a polythioether backbone bearing pyridylamino groups are first synthesized by the amination of poly-chloromethylthiirane with various aminopyridine (i. e. 2-aminopyridine, 3-aminopyridine and 4-aminopyridine) by using diethylenetriamine as the crosslinking agent. These resins cheJate strongly with Ag( Ⅰ ), Au( Ⅲ ) and Pd( Ⅱ ), moderately with Pt(Ⅳ), Hg( Ⅱ ) and Cu( Ⅱ ), as well as weakly with Zn( Ⅱ ) and Cd( Ⅱ ), whereas Pb( Ⅱ ) could not be chelated. PTAPresins possess excellent selectivity for noble metal ions. Au(3) or Pd( Ⅱ ) is only adsorbed from the solution of salts including Au( Ⅲ ) or Pd( Ⅱ ), Zn( Ⅱ ), Hg( Ⅱ ) and Cd( Ⅱ ) etc. In addition, from the mixed solution of PdCl
2
and H
2
PtCl
6
Palladium( Ⅱ ) is adsorbed, but platinum(Ⅳ ) can hardly be adsorbed. The influence of acidity of medium on adsorption efficiency of PTAP for Au( Ⅲ ), Pd( Ⅱ ), Pt( Ⅳ ) is also investigated.
Dchydrochlorination of Polyvinylchloride-Phase Transfer Catalyst Film in Aqueous Sodium Hydroxide Solution
Wang Rongshun, Xie Demin, Fu Yujie, Zhang Xiyan, Wang Yusong, Zhao Chengda
1990, 11(5): 516-520.
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The solution of polyvinylchloride with a phase transfer catalyst-tetrabutylammonium bromide (TBAB) was casted into film, then it was immersed in aqueous sodium hydroxide solution for de-hydrochlorination. The structure of the product was characterized by FTIR and UV-VIS spectropho-tometry. Comparing with Kise's method we found that the elevated extent of reaction rate and conversion in the system of PVCwas more remarkable than that in the system of PVDF, and a considerable concentration of very long trans-(CH)
x
, chain sequences was induced. We studied the effects of temperature, time and the quantity of catalyst used on the reaction and the best reaction condition was obtained.
Studies on the Preparation and Hydrogenation Properties of Polymer Supported Colloidal Palladium Catalysts
He Binglin, Sun Juntan, Li Hong, Jin Xiaonong
1990, 11(5): 521-525.
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Several polymer supported colloidal palladium catalysts were prepared and characterized by infrared, X-ray diffraction analysis, scanning electron micrograph. The above mentioned catalysts were used to catalyze the hydrogenation of 1,5,9-cyclododecatriene and other unsaturated compounds under the reaction conditions of temperature 80～100 ℃, hydrogen pressure 196.133×10
4
Pa by using benzene-ethanol as a mixed solvent. The catalytic activity, selectivity, reproducibility and the influence of reaction conditions on the properties of the catalysts were studied.
Studies on the Colour-Producing Reactions of Alkaline Earth Metals with Polyhalogcnated Bisazo Derivatives of Chromotropic Acid Containing-PO
3
H
2
Zhao Yeping, Ren Ying, Yu Ximao
1990, 11(5): 526-528.
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The title reagents can form colour complexes with alkaline earth metal. In this paper, the absorption spectrum, the optimum ranges of acidity, the sensitivity and selectivity for the colour reactions of these reagents with alkaline earth metal as well as the composition of complexes were studied. Both Chlorophosphouazo-TB and Chlorophosphouazo-DBC are excellent Chromogenic reagents in the spectrophotametuc determination of strontium, barium and calcium.
Studies on A. C. Oscillopolarogram ( Ⅲ ) —— The Modification of Micka's Equation in Solution Containing Only Supporting Electrolyte
Bi Shuping, Gao Hong(H. Kao)
1990, 11(5): 529-531.
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Micka's equation is modified by using the conception of direct current potential to explain the influence of d. c. potential on the A. C. oscillopolarogram. The theoretical conclusion are qualitatively confirmed through experimental work.
Syntheses of 3,4-Dihydro-4-Oxopyrimido[4,5-b]Quinolines
Chen Wei, Jiang Guiji
1990, 11(5): 532-533.
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Syntheses of N-Substituted 3, 4-dihydro-4-oxopyrimido[4, 5-b]quinolines which were achieved by reaction of N-Substituted 2-aminoquinoline-3-carboxyamides with formamide are described in detail. The structures of 20 new compounds have been confirmed by element analysis, IR and
1
H NMR.
The Synthesis of O-Ethyl-O- (Substituted y-Butyrolactonylenyl-methyl) N-Alkyl (or N,N-Dialkyl) Phosphoramidothioatcs
Chen Ruyu, Zeng Qiang, Duan Jianrong
1990, 11(5): 534-536.
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In this paper, a series of new compounds were prepared by the reaction of O-ethyl-N-alkyl (or N,N-Dialkyl amidothiophosphoryl chloride with several sodium salts of a-hydroxymcthylene lac-tones in the presence of DMAP. The structure of these new compounds were confirmed by elemental analysis,
1
H NMR,
13
C NMR, and so on. The isomerization of them had been studied. Most of the compounds have fungicidal activities at 500 ppm. They have plant growth regulation activites.
Synthesis of Ranunculin
Wang Zhongqi, Chen Yi, Wu Yuehuan, Zhu Zhouyuan
1990, 11(5): 537-539.
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This article reports that main intermediate (S)-4-triphenylmethoxymethyl-Δ
2
-butenolide (4d) is produced from L-giutamic acid through four step reactions and target Ranunculin(1) is obtained by the known methods after 4d turn into (S)-4-hydroxymethyl-Δ
2
-butenolide (4a).
An ESRtudy on Quinone Radical Anions Formed by the Reaction of Ascorbic Acid with Quinones
Zhang Fa, Fang Huai, Chen Wei, Liu Zhongli, Liu Youcheng
1990, 11(5): 540-542.
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Quinone radical anions of p-benzoquinone, 2,5-dimethyl-, 2,6-dimetiiyl-,tert-butyl-, and 2,6-di-tert-butyl-p-benzoquinones, 1,4-naphthaquinone and 2-methylnaphthaquinone were detected by ESR in a water-DMSO mixed solvent with pH = 8. 5 when the corresponding quinones reacted with ascorbic acid. The results were rationalized by the single electron transfer reaction between the quinone and ascorbic acid.
Synthesis and Antitumor Activity of Amino Acid 5-Fluorouracil-1,3-dipropyl Esters Hydrochloride
Zhao Rulin, Fan Changlie, Zhuo Renxi
1990, 11(5): 543-545.
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Ten amino acid 5-fluorouracil-1,3-dipropyl esters hydrochloride were obtained by the reaction of N-protected salts of amino acid with 1,3-bis(w-bromopropyl)-5-fluorouracil in the DMF and then deprotecting with HCl-MeOH. The structures of these new compounds were characterized by
1
H NMR, IR and UV spectra as well as elemental analysis. The antitumor activities of all of the compounds were tested against EAC in vitro, the preliminary results showed that some of the compounds exhibit certain anititumor activity.
Computer Simulation of the Structure of Cryolite-alumina Melts
Xie Qang, Qiu Zhuxian
1990, 11(5): 546-547.
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Monte Carlo simulation calculation with an elctronic computer was performed on melts of cryolite-alumina. The characterization of the local structure and radial distribution functions of the molten salt were computed at 1283 K. In the melt Al
3+
ions tended to have a preferential averaged coordination number of 3. 4F
-
. It is found that there exist complex ionic AlF
4
-
,AlF
5
2-
,and AIOF
3
2-
, AlOF
2
-
etc. There also exist oxygen-bridge [AlF
3
- O - A1F
3
]
2-
and flourine-bridge [F
3
A1- F -A1F
2
]
-
ionic clusters due to the mutual reactions among various species in the molten salt.
Composition and Sensitivity to pH of Palladium Oxide Electrodes Prepared by Thermal Oxidation
Wu Baozhang, Wu Huihuang
1990, 11(5): 548-550.
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Thermal oxidation of Pd in air was studied by thermogravimetric analysis. The composition and properties of the palladium oxide electrodes prepared at different temperatures were characterized by using XPS and electrochemical methods. It is found that the pHresponse of these electrodes depends strongly on the preparation temperature, and Pd( Ⅳ ) oxide is essential to a better pHrespone. The pH-sensing mechanism .was also discussed.
Studies on the Thermodynamic Properties of Adduction Reaction between Ni[(C
8
H
17
O)
2
PS
2
]
2
and Aldehydes by GLC Method
Yu Yunpeng, Zhu Duolin, Xu Zheng, Lin Jianhua, You Xiaozeng
1990, 11(5): 551-553.
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The thermodynamic properties of adduction reaction of Ni[(C
8
H
17
O)
2
PS
2
]
2
and CH
3
CHO, C
2
H
5
CHO, n-C
3
H
7
CHO and n-C
4
H
9
CHO were studied by GLC method. The equilibrium constants were determined between 333～363K and described by the emperical equation: 1gK = - 0.2087 - 0. 9209 N
c
+ (291. 9 + 265. 1 N
c
)/T ΔH and ΔS were calculated by the least square method. It was found that - ΔH and - ΔS increased linearly with the increase of number of carbon in aldehydes: -ΔH=5. 59 + 5. 08 N
c
(kJ/mol), -ΔS=3. 39 + 17. 63 N
c
(J/K ·mol). The nature of adduct bonds was explained by electro-static model.
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