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Table of Content
24 December 1994, Volume 10 Issue 4
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Articles
Synthesis, Crystal Structure and Thermode-composition Kinetics of Copper(Ⅱ) Complex with bis-(Schiff base)Derived from 3-Methoxysalicylaldehyde and Ethanolamine
LI Shu-lan, WANG Hong, LIU De-xin, MENG Fan-qin, YANG Zhao-he
1994, 10(4): 273-279.
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The present paper covers the synthesis,crystal structure and thermodecom-position kinetics of bis [(3-methoxysalicylal)-ethanolamine] copper (Ⅱ) complex.X-ray diffraction determination gave the following crystal data: triclinic system.space group P1,Z=2.a = 0.8841 (4).b =1.0773 (2), c = 1.1321 (3) nm.α=70.38(1),β= 70.70(2).γ=78.29 (2)°.The final agreement factors were R =0.075, R
w
= 0.067, respectively.Investigation on non-isothermal kinetics of thecomplex favored second order kinetics.The kinetic equation is expressed as: da/dt= A × e
-E/RT
×(1 -α)
2
.
Application of the Reactions of Ferrocene(Ⅰ) Saltswith Bis [dicarbonyl (η
5
-cyclopentadienyl) iron]and Bis [dicarbonyl (η
4
-butadiene) cobalt]Complexes to Organic Synthesis
TAO Ke, WU Le, Wurenqimug, YANG Wan-zheng
1994, 10(4): 280-284.
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Complexes[(η
5
-C
5
H
5
)Fe (CO)
2
L]
+
BF
4
-
(Ⅱ)[L=PPh
3
,P(OPH)
3
,P(OC
2
H
5
)
3
,pyridine, 3-acetyl-pyridine, 4-methyl-pyridine, phenyl cyanide, quinoline] and[(η
4
-C
4
H
6
)Co(CO)
2
L]
+
BF(Ⅱ)[L=PPh
3
,P(OPH)
3
,P(OC
2
H
5
)
3
],were respec-tively produced in the reactions of[(η
5
-C
5
H
5
)Fe (CO)
2
]
2
and [(η
4
-C
4
H
5
)Co(CO)
2
]
2
with Cp
2
FeBF
4
in the presence of the ligands.Some characteristics of these reac-tions were discussed and all the complexes were identified by IR and
1
H NMR spec-troscopy.These complexes are air-stable and the preparative metliods are simple.
Isolation and Structure Elucidation of New Glycosides from the Leaves of
Oplopanax Elatus Nakai
(Ⅱ)
WANG Guang-shu, ZHAO Chun-fang, XU Jing-da, Tetsuya Murayama, Junzo Shoji
1994, 10(4): 285-290.
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Again, four new saponins were isolated from tlie leaves of Oplopanax elatusHaka,.The structures of the four saponins ,tentatively named cirensenoside E(1),F(2), G(3) and H(4),were elucidated to be 28-O-α-L-rlianinopyranosyl(1→4)-β-D-glucopyranosyl(1→6)-β-D-g-Dglucopyranosyl esters of 3epi-betulinic acid 3-O-β-D-glucopyranoside (1), 3β-hydroxylup-20 (29)-en-23.28-dioic acid (2),3β, 23-di-hydroxylup-20 (29)-en-28-oic acid (3), 3α, 23-dihydroxylup-20 (29)-en-28-oic acidt4), respectively.
Off-line Two-Dimensional Gas Chromatography-Mass Spectrometry for Analysis of EssentialOil of Medicinal Herb──Use of Absorption Trap
MA Xue-yi, PAN Hui-ping, CHEN Yao-zu
1994, 10(4): 291-296.
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The use of an absorption trap off-line two-dimensional gas chromatography (2-DGC) in conjunction with a mass spectrometer greatly improved the separation andidefitification of minor constituents of a complex mixture such as a natural essentialoil.The absorption trap device used as an interface of 2-DGC offered the advantageof convenient manipulation.
Quantitative Determination of BenoxinateHydrochloride by Three Wavelength Spectrophotometry
HUI Rui-hua, HOU Dong-yan, HUI Yu-lin
1994, 10(4): 297-300.
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Three wavelength spectrophotometry was used to determine the content ofbenoxinate hydrochloride.Using this method could effectively eliminate the devia-tion of background absorption caused by the change of concentration and the errorof quantitative anaiysis caused by asymmetric peaks, and at the same time the lean-ing degree of base line was corrected.This method was simple, the recovery was 98.62% 101.86% and the coefficient of variation was 0.551%.
Piezoelectric Fiber-optic Spectroelectrochemistry──A New Technique of Spectroelectrochemistry inCombination With Piezoelectric Quartz Crystal Detection
XIE Qing-ji, HE Feng-jiao, NIE Li-hua, YAO Shou-zhou
1994, 10(4): 301-307.
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Piezoelectric fiber-optic spectroelectrochemistry(PFOSEC), a new techniqueof spectroelectrochemistry (SEC)in combination with piezoelectric quartz crystal(PQC)detection is proposed.In this technique, one arm of a bifurcated fiber-opticprobe is used to conduct the incident light beam to the investigated solution andthen to the reflective electrode surface on the piezoelectric quartz crystal, and thereflection light beam is guided to the optical detector by the other arm of the opticfiber.Atypical experiinental system, Cu(Ⅱ)in glycine and KNO
3
supporting elec-trolyte, was used here to test this new technique.Results show that this techniquecan provide substantial in situ information from SEC, PQC and conventional elec-trochemistry in the investigation of the electrochemical process.This novel techiqueis recommended to find wider application in the electrochemical study not only onsolution species but also on surface phenomena.
Synthesis and Crystal Structure of[(2,4-Me
2
C
5
H
5
)
2
NdC＝CC
6
H
5
]
2
ZHANG Suo-bo, LIU Ju-zheng, WEI Ge-cheng, JIA Heng-qing, CHEN Wen-qi
1994, 10(4): 308-312.
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The reaction of (2,4-C
7
H
11
)
3
Nd with HC＝CC
6
H
5
in toluene leads to [(2, 4-C
7
H
11
)
2
NdC＝CC
6
H
5
]
2
,which crystallizes in the space group P
cab
with unit cell pa-rameters a=1.0489 (11), b=1.8033 (12), c=2.1064 (15)nm and Z=4,least-squares refinement based on 2323 observed reflections converged to a final Rvalueof 0.08.The molecular structure shows that the complex is a dimer, in which two(2,4-C
7
H
11
)
2
Nd units are connected by asymmetrical alkynide bridges with indepen-dent Nd-C(alkynide) bond lengths of 0.2552(25)and 0.2560(24)nm, Nd-C=Cangles of 124.1(17)° and 134.2(17)°.
Preparation and Characterization of LacunaryHeteropolymolbdophosphates Coordinated with Divalent Metal Ions of the Fourth Period
QIN Du-jie, WANG Guo-jia, WU Yue
1994, 10(4): 313-320.
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The present paper covers tlie preparation and isolation of a series of monosub-stituted molybdophosphates Na
5
[PZ(H
2
O)Mo
11
O
39
]·5H
2
O (Z=Mn
2+
, Co
2+
,Ni
2+
, Cu
2+
, Zn
2+
)by an improved method.These complexes were characterized byfull elemental analysis, IRspectra and UV-Vis.The studies show that the pre-pared products still keep Keggin structure and the substituting metal would belooated in coordination site.Based on this, their some pysico-cliemical propertiesrelated with their catalytic beliaviour,such as thermal stability and acidity proper-ty, were studied.
Deactivation of Ti-La-Li Multicomponent OxideCatalyst for Oxidative Coupling of Methane
ZHAO Zhen, YUAN Song-yue, YU Zuo-long
1994, 10(4): 321-326.
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The deactivation of highly active multicomponent oxide LiLa
0.5
Ti
0.5
O
2+λ
cata-lyst at high reaction temperatures has been studied.The surface and bulk structureof the catalyst were characterized by means of XRD, IR, XPS, BET, O
2
-TPD,SEM etc..The results show that the deactivation of the catalyst at high reactiontemperatures is mainly due to the loss of surface lithium.As a result,the diffusionof lithium from bulk to surface leads to the decompositiqn of the active phase con-taining lithium, which lowers tlie number of oxygen vacancies and decreases themobility of lattice oxygen.
Initiation Mechanism of Polymerization of Acryl-amide by Ceric Ion/2-Benzoyl Acetanilide System
DONG Jian-hua, DENG Chao, QIU Kun-yuan, FENG Xin-de
1994, 10(4): 327-332.
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The initiation mechanism of ceric ion/2-benzoyl acetanilide system was studiedby means of FT-IR, EPR and kinetic studies which revealed that 2-benzoyl ac-etanilide acts as a very active promotor to the polymerization initiated by ceric ion.The initiation mechanism was then proposed which involved the complex formationbetween a ceric ion and a l, 3-diketone group or a carbamate group, followed by,thedecomposition of the complex to generate C-centered secondary alkyl radical and N-centered anillido radical, both of which would initiate polymerization of vinylmonomer as the end groups of the polymers formed.
Preparation of CaZrO
3
Powder Through Oxalate Precipitation Route
ZHENG Wen-jun, LIU Chuan, PANG Wen-qin, XU Shan-peng
1994, 10(4): 333-334.
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A New Diterpene Ester from
Euphorbia Aleppica
SHI Yan-ping, JIA Zhong-jian, YANG Li, SALEH Sadiq A., LAHHAM Jamil
1994, 10(4): 335-337.
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(η
2
C
60
)Pt (PPh
3
)
2
as the Catalystfor the Hydrosilylation of Olefins
CHEN Yuan-yin, SHENG Rong-shen, LIU Ying
1994, 10(4): 338-340.
Abstract
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)
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Metal Complexes of Antibiotic Pipemidic Acid
QIAO Ben-zhi, LU Yun, XUAN Chong-sheng
1994, 10(4): 341-347.
Abstract
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)
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Studies on Some Gadolinium(Ⅲ) Complexes asNew Water-Soluble Paramagnetic RelaxationReagents(RR) for
13
C NMR Spectrometry
WANG Ying-zi, ZHAO Da-qing, REN Ji-min, NI Jia-zan
1994, 10(4): 348-352.
Abstract
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)
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Synthesis and X-ray Structure of a BinuclearNickel (Ⅱ) Complex of Nickel (Ⅱ)Perchlorateand 2,2'-Bipyridyl with N, N'-Bis (2-aminoethyl)oxamido Nickel (Ⅱ)
LIU Chang-rang, JIA Lu, WEI Ping-rong, FAN Yao-ting, HAN Qiang
1994, 10(4): 353-359.
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)
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Analysis of the Volatile Constituents of PinusTabulaeformis Carr. Pine Cones
ZHANG Wei-hua, HOU Dong-yan, HUI Rui-hua, JING Run
1994, 10(4): 360-363.
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)
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Synthesis of Benzoxepinoquinolinone Derivatives
GAO Yong-jun, LI Chun-jie, ZAO Hua, JIANG Ri-shan, JIANG Gui-ji
1994, 10(4): 364-368.
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)
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Synthesis of α-Oxoketene Cyclic O,S and S,S Acetals
LIU Qun, XU Bai-ling, ZHAO Hong-wu
1994, 10(4): 369-372.
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)
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Studies on the Synthesis and Crystal Structure of 5-(3'-methylphenyl)-2H-tetrazol-2-ylacetic acid
ZHANG Zi-yi, ZOU Ning
1994, 10(4): 373-376.
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)
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A Raman Study of the Effect of TrivalentLanthanide Ions on the Conformational Disorderin Acyl Chains of Phospholipid Bilayers
YUAN Chun-bo, ZHAO Da-qing, NI Jia-zuan, ZHAO Bing, Hwang Fen
1994, 10(4): 377-380.
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)
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Oxidative Dehydrogenation of Isobutaneto Isobutylene over F
-
Modified RareEarth Metal Oxide Catalysts
ZHANG Wei-de, TANG Ding-liang, LAI Wen-qang, WAN Hui-lin, K. R. TSAI
1994, 10(4): 381-383.
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Editor-in-Chief:
Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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