Chemical Research in Chinese Universities

Syntheses and Characterization of ZSM-5 Zeolites Containing Diethylamine and Ethylenediamine

ZHAO Da-qing, QIU Shi-lun, PANG Wen-qin

1993, 9(2): 95-98.

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Syntheses of ZSM-5 zeolites from R-SiO₂-Al₂O₃-H₂O-HF(R = diethylamine and ethylenediamine, respectively) were investigated by using the hydrothermal crystallization. The large single crystals of ZSM-5 containing diethylamine and ethylenediamine were synthesized. The ZSM-5 precursors were characterized by means of X-ray powder diffraction, scanning electron microscopy, thermal analysis and electron microprobe analysis. The analysis result of aluminium distribution shows that the interior aluminium content of large crystals of ZSM-5 zeolites is rather low.

Studies on Synthesis, Structure and Properties of Cobalt Complex [Co(Ⅰ) (dppe)₂CO]₂[Co₂(Ⅱ) (dppe)Cl₆O₂]

WANG Tao, FAN Yu-guo

1993, 9(2): 99-103.

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Acobalt complex with mixed valence state [Co(Ⅰ) (dppe)₂CO]₂ [Co₂ (Ⅱ)(dppe) Cl]₆O₂] (dppe=1,2 -bis(diphenylphosphino) ethane) has been prepared. The compound crystallizes in triclinic space group P1 with unit cell parameters: a=1.1763(3)nm, b=1.2943(6)nm, c=2.1507(9)nm, a=81.44(4)°,β=82.58(3)°, r=79.82(3)°, V=3.1691nm³ and Z=1. The structure was solved by direct method according to ALPHAcriterion and was refined by a block diagonal matrix least-squares procedure to final R= 0.084, Moreover, infared spectra, electronic reflection spectra and cyclic voltammetry curve were mearsured.

Higher Order Cuprate Species(Ⅱ)——Stereospecific Carbocupration of Terminal Alkynes and Its Synthetic Utility for (±)-Ipsenol and (E)-β-Farnesene

PAN Yi-jun, XU Zhang-huang, CHEN Jia-wei, SUN Dong-chen

1993, 9(2): 104-109.

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The stereospecific carbocupration of terminal alkynes via higher order cuprates to give 1,1’-disubstituted olefins with 99% configuration purity is described. Its synthetic utility as a general method for the preparation of substituted olefins is further illustrated by the direct synthesis of (±)-ipsenol and (E)-β-farnesene with highly geometric purity of the carbon-carbon double bond.

The i-E Equations of Steady-state Voltammograms at Microdisk Electrodes

ZHUANG Qian-kun, CHEN Hong-yuan

1993, 9(2): 110-115.

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Based on the theories of conventional electrodes, as well as the properties of microdisk electrode, the i-Eequations for chronoamperometry at disk microelectrode for reversible, quasi-reversible and irreversible systems are derived. Steady-state voltammograms for the oxidation of [Fe(CN)₆]^4-, Fe²⁺ and ascorbic acid were measured at a series of microdisk electrodes with different radii. The conventional log-plot shows that oxidations of [Fe(CN)₆]^4- and ascorbic acid are reversible and totally irreversible, respectively, but the oxidation of Fe²⁺ is reversible at larger radius microdisk electrodes and quasi-reversible at smaller radius microdisk electrodes. The application of the log-plot to the voltammograms yielded a straight line, its slope allows us to evaluate the charge transfer coefficient and the intercept gives values of the electron transfer rate constant.

Anticancer Drugs (Ⅳ)——New Derivatives of Podophyllotoxin

TIAN Xuan, LI Jin-xin, ZHANG Ya-li, CHEN Yao-zu, LI Wen-guang

1993, 9(2): 116-120.

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Four new derivatives of podophyllotoxin, N’-podophyllic acid-N-[3-(2, 2, 5, 5-te-tramethyl-pyrrolinenyloxy)] semicarbazide(GP-11, 6), podophyllic acid [3-(2,2,5,5-te-tramethyl-pyrrolinenyloxy)]hydrazone (GP-12, 7), podophyllic acid-[4-(2, 2, 6, 6-tetramethyl-1-hydroxy piperidine)]hydrazone(GP-1-OH, 8) and podophyllic acid[4-(2,2, 6, 6-tetramethyl piperidine)]hydrazone(GP-1-H, 9) were synthesized. The inhibition effect of the four new compounds on L-1210 cells were determined. The antitumor activity and toxicity of GP-1(2), GP-1-OH(8), GP-1-H(9) and VP-16-213(1) were discussed.

Studies on Silicon-Containing Fragrance Raw Materials(Ⅱ)——Syntheses and Odors of 4-Trimethylsilylcyclohex-3-enol and 4-Trimethylsilylcyclohexanol Derivatives

TANG Shi-xiong, XUE Jie-you, WU Jun-jun, CAO Yu-rong, ZHI Jin-fang, WANG Xiao-lan

1993, 9(2): 121-126.

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1-Substituted- 4-trimethylsilylcyclohex- 3-enol and 1-substituted- 4-trimetnylsilyl-cyclohexanol, 4-trimethylsilylcyclohex-3-enol and 4-trimethylsilylcyclohexanol, and some of their esters and carbon counterparts were synthesized. Structures of the nineteen new compounds were determined by ¹H NMR, IRand MS. Their odors are evaluated.

Studies on Silicon-Containing Fragrance Raw Materials (Ⅳ)——Synthesis of Spiro-Acetals of 5-Trimethylsilylcyclohex- 2- (or 3)enone

TANG Shi-xiong, XUE Jie-you, DUAN Mao-sheng, CAO Yu-rong, ZHI Jing-fang, WANG Xiao-lan

1993, 9(2): 127-132.

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Some novel spiro-acetals of 5-trimethylsilylcyclohex-2(or 3)-enone were synthesized from the reaction of silylcyclohexenones with the corresponding a, ω-diols in the presence of oxalic acid or adipic acid.

Synthesis, Structure and Properties of Co(NH₂CSNHNH₂)₃Cl₃·1/2HCl

LI Shu-jia,NIU Shu-yun, ZHANG Heng-bin, YANG Guang-di, LI Li, NIE Fu

1993, 9(2): 133-138.

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The single crystal of title compound was obtained in the solution of DMFand CH₃OHunder the radiation of IRlamp. The crystallographic parameters obtained are as follows: trigonal system, space group P31C, Z=4, a=b=1.0008(2)nm, c=2.4011 nm; final R=0.099, R_w=0.092. The properties of title compound were characterized by IR, UV, EPR, XPSand CVmeasurements.

Crystal Structure of [Et₄N][Sm(S₂CNEt₂)₄]

SUN Chun-ting, WANG Chai-xia, HUANG Qi-jun, LANG Xi-guang,ZHU Ya-bin, LU Gong-xian, WEI Ge-cheng, JIN Zhong-sheng, LIU Yong-sheng

1993, 9(2): 139-142.

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The crystal structure of .[Et₄N][Sm(S₂CNEt₂)₄] was determined by X-ray diffraction technique. The crystal crystallizes in monoclinic system, space group P2₁/n with a= 1.1695(3), b=2.0821(6), c=1.7420(7)nm, β=99. 79(3)°, Z=4, D_c= 1.39g/cm³, μ(Mo/KTσ) = 18.4cm^-1, F(000)=1812. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional Rof 0. 053 for 3116 (Ⅰ> 3σ-(Ⅰ)) reflections. Each asymmetric unit contains two ions [Sm (S₂CNEt₂)₄]^-1 and [Et₄N]⁺¹, having distance between central atoms N5 and Sm³⁺ to be 0.6522nm. The atom Sm is coordinated by eight sulphur atoms. The Sm-Sdistance lies in the range of 0.285-0.290nm with an average of 0.288nm.

Synthesis of Liquid Crystalline Polymers with Side Chains

YANG Chun-cai, ZHAO Dong-hui, TANG Xin-yi, FENG Gui-zen

1993, 9(2): 143-147.

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The present paper covers the synthesis and characterization of several intermediate products, monomer, and polymers. 3-{ 2-[ 4-(4-Nitrophenylazo) phenoxy] ethyloxycarbonyl} propanoyloxy (2-hydroxy) propyl acrylate (4) was prepared by the ring-opening reaction of glycidyl acrylate with the monoester of succinic acid (3). The polymers (5) with different molecular weights were prepared by the free-radical polymerization. The polymers (5) had liquid crystalline behavior without decomposition as revealed by DSC, optical microscope.

The Polymerization of Methyl Methacrylate in the Presence of a New Homogeneous Yttrium Catalyst

LIU Jian-fei, SUN Jun-quan, SHEN Zhi-quan

1993, 9(2): 148-151.

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Methyl methacrylate(MMA) polymerized in the presence of a new homogeneous catalyst of Y(acac)₃-(i-Bu)₃Al-BuLi. The effects of MMA/Y, Al/Y, Li/Ymolar ratios, polymerization temperature and time are reported. The results show that a small amount of butyl lithium could greatly enhance the activity of the catalyst and the polymerization reaction could be carried out at low temperatures (-25℃-10℃) with a high conversion. 200 kg of poly(methyl methacrylate) (PMMA) with 63% syndiotacticity could be prepared by using 1 mole of yttrium.

Total Syntheses of (+)-Goniotriol and (+)- 8-Acetylgoniotriol

ZHOU Zhao-hui, SHING T. K. M.

1993, 9(2): 152-153.

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Hypersensitive Spectrophotometric Determination of Trace Amounts of Tin (Ⅳ) with Salicylfluorone and Mixed Surfactants

XIE Zeng-hong, WANG Dong-jin, ZHOU Xue-ying, HU Xian-guo

1993, 9(2): 154-160.

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