2003 Volume 14 Issue 9

New Stereoselective Synthesis of 4-Butyl-α-agarofuran
Chun LI , Da Li YIN , Hui Qin HUANG , Xiang Hong WU , Ji Yu GUO
2003, 14(9): 881-882
[Abstract](170) [FullText HTML] [PDF 750KB](1)
Abstract:
A potent anxiolytic 4-butyl-α-agarofuran (AF-5) was synthesized from (+)dihydro-carvone.Acid catalyzed hydration of (+)dihydrocarvone and interconversion with β-O-ketone 8 and the key intermediate α,β-unsaturated ketone 5 made this synthesis more practical.
The Synthesis of Cyclic Amino Acids
Shrong Shi LIN , Jing yuan LIU , Jian Mei WANG
2003, 14(9): 883-884
[Abstract](199) [FullText HTML] [PDF 695KB](3)
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Several cyclic amino acids(1-4)were synthesizedfrom glycine.Isocyanate ester wasprepared asthe keyintermediate and reacted with dibromoalkanesto affordthetarget compounds.
Convenient Solid-phase Synthesis of Benzothiazole Derivatives
Jing TANG , Lu Ling WU , Xian HUANG
2003, 14(9): 885-886
[Abstract](181) [FullText HTML] [PDF 750KB](0)
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Resin-bound cyclic malonic ester 1 reacted with aryl isothiocynate, then was treatedwith bromine, followed by cleavage from the resin under perchloric acid to give benzothiazoles 4.
A Stereoselective Synthesis of Substituted Allyl Alcohol by Three-component Rection of Acetylenic Sulfone, Phenylseleno-magnesium Bromide and Ketones
Mei Hua XIE , Lu Ling WU , Xian HUANG
2003, 14(9): 887-888
[Abstract](165) [FullText HTML] [PDF 757KB](0)
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Phenylseleno and sulfonyl substituted allyl alcohols were synthesized stereoselectively by the three-component reaction of acetylenic sulfone, phenylselenomagnesium bromide and ketones in one-pot.
Studies on the Model Synthesis of the Brassinolide and Dolicholide Side Chains
Li Zeng PENG , Feng Zhi ZHANG , Tian Sheng MEI , Yu Lin LI
2003, 14(9): 889-892
[Abstract](161) [FullText HTML] [PDF 1355KB](0)
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A stereoselective synthesis of brassinolide and dolicholide, which involves construction of the side chain enantiomers by a highly stereoselective aldol reaction of aldehyde 5 with the anion of α-silyloxy ketone 6 is described.
A Facile and Efficient Synthesis of Substituted Pyrroles by Three Component Coupling Reaction of Amines, Aldehydes and Nitroalkanes
Yi Song XIAO , Yan Guang WANG
2003, 14(9): 893-896
[Abstract](170) [FullText HTML] [PDF 1421KB](0)
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A facile and efficient synthesis of highly substituted pyrroles has been achieved by a one-pot three-component coupling reaction of aldehyde, amine and nitroalkane by triethyl orthoformate.
Synthesis and Herbicidal Activities of 3-(Substituted phenyl)isoxazole Derivatives
Yu Han ZHOU , Wei Rong MIAO , Lu Bai CHEN
2003, 14(9): 897-900
[Abstract](165) [FullText HTML] [PDF 1411KB](0)
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Several novel 3-(substituted phenyl)isoxazole derivatives were prepared from phenylbutan-1,3-dione.Their structures were confirmed by 1H NMR, IR, and CIMS.Preliminarybioassay showed that some of them exhibited good activities toward various weeds.
Synthesis and Characterization of Novel N-Ferrocenesulfonyl Benzimidazole
Bing Qin YANG , Peng Hui YANG , Ai Lin ZHU
2003, 14(9): 901-903
[Abstract](165) [FullText HTML] [PDF 957KB](0)
Abstract:
A new series of ferrocenesulfonyl benzimidazle has been synthesized and characterized by 1H NMR, FT-IR and elemental analysis.They are expected to have special bio-activity.
Microwave-assisted Regioselective 1-O-Deacylation of Peracylated Glycopyranoses on Alumina
Jia Qiang DONG , Shu Jia ZHANG , Yan Guang WANG
2003, 14(9): 904-906
[Abstract](155) [FullText HTML] [PDF 1037KB](0)
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A facile, rapid and regioselective method for the l-O-deacylation of peracylatedglycopyranoses is described which occurs under mild conditions by absorption onto alumina usingmicrowave irradiation.
The Studies of the Reactions of 2, 4, 6-Triphenylpyrylium Tetrafluoroborate with Amino Acids
Shrong Shi LIN , Xian Jing KONG , Jing Yuan LIU , Cheng Yong LI
2003, 14(9): 907-910
[Abstract](195) [FullText HTML] [PDF 1434KB](7)
Abstract:
The reactions of triphenylpyrylium salt 1 with various amino acids were explored andcompared.The reactions with most α-amino acids yielded decarboxylation products 2 viadecarboxylation.The reactions with glutamic acid, lysine and ACC (1-aminocyclopropyl-carboxylic acid) gave triphenylpyridine 8, dimer 9 and acid 5a-acc, respectively.The reactionswith β and γ-amino acids yielded triphenylpyridine by intramolecular elimination.
Copolymerization of Ethylene/1-Butene with Heterogeneous TiCl4/(α-Diimine)nickel(Ⅱ) Complex Combined Catalyst
Shao Quan LIN , Qi Xing ZHANG , Hai Hua WANG
2003, 14(9): 911-913
[Abstract](175) [FullText HTML] [PDF 887KB](1)
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The new type heterogeneous combined catalyst system TiCl4-(α-diimine)nickel(Ⅱ) complexes/MgCl2-SiO2/AlR3was prepared.Ethylene and 1-butene were copolymerized with thecatalysts in slurry phase.It was found that with combined catalyst, the copolymers with lowerdensity and higher branched degree were obtained.13CNMR results showed that in the obtainedcopolymers existed not only ethyl but also some other kinds of branches due to the fact thatethylene exhibits the behavior of oligomerization and copolymerizafion in-situ with combinedcatalysts.
Synthesis and Adsorption Property of Two Polymeric Adsorbents with Pendent Ether Bonds
Jian Gou HUANG , Man Cai XU , Hai Tao LI , Zuo Qing SHI , Bin Lin HE
2003, 14(9): 914-916
[Abstract](155) [FullText HTML] [PDF 1296KB](0)
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Two polymeric adsorbents, poly(methyl p-vinylbenzyl ether) and poly(phenyl p-vinylbenzyl ether), were synthesized from chloromethylated polystyrene.Their adsorption property for phenol in hexane solution was investigated.The results showed that the two adsorbents adsorb phenol from hexane solution through hydrogen-bonding and π-π stacking interaction.
Aqueous Biphasic Hydroformylation of Oleyl Alcohol Catalyzed by Thermoregulated Rhodium Complex
Fan Zhi KONG , Xiao Lai ZHENG , Zi Lin JIN
2003, 14(9): 917-919
[Abstract](164) [FullText HTML] [PDF 1020KB](0)
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The aqueous biphasic hydroformylation of oleyl alcohol was achieved under thermo-regulated phase transfer catalysis (TRPTC) conditions with Rh(acac)(CO)2 Ph2P[p-C6H4(OCH2CH2)25OH] (PETPP) complex catalyst formed in situ.The aldehyde yield reached 81.2% within 6 hrs under 140℃ and 5.0 MPa (CO/H2,1/1) and the separated catalysts dissolved in the aqueous phase could be reused for 3 times without evident changes in activity.
A New Flavonol Diglycoside from Pyrrosia petiolosa
Yong Chun YANG , Chun YANG , Shun Yan MO , Jian Gong SHI
2003, 14(9): 920-922
[Abstract](174) [FullText HTML] [PDF 995KB](0)
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A new flavone diglycoside, named as pyrropetioside A 1 was isolated from Pyrrosia petiolosa.Its structrue was elucidated as 7-O-[6-O-(α-L-arabifuranosyl)-β-D-glucopyranosyl]-gossypetin by means of chemical and spectroscopic methods including IR, MS, 1D and 2D NMRtechniques.
Two New Flavonol Glycosides from Daphniphyllum oldhami
Yu Bo WANG , Shuang Xi MEI , Yao Hua WANG , Jing Feng ZHAO , Hai Ying REN , Jie GUO , Hong Bin ZHANG , Liang LI
2003, 14(9): 923-925
[Abstract](168) [FullText HTML] [PDF 882KB](0)
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Two new flavonol glycosides (1 and 2) together with two known flavonoides (3 and 4),were isolated from the whole plant of Daphniphyllum oldhami willd.The structures of 1 and 2 were elucidated as kaempferol-7-O-α-L-arabinosyl-3-O-β-D-6"-acetylglucopyranoside and kaempferol-7-O-α-L-arabinosyl-3-O-β-D-3",6"-diacetylglucopyranoside respectively.
A New Flavan-3-ol Glucoside from Daphniphyllum oldhami
Zhi Yu SHAO , Da Yuan ZHU , Yue Wei GUO
2003, 14(9): 926-929
[Abstract](163) [FullText HTML] [PDF 1266KB](0)
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A new flavan-3-ol glucoside, (-)-afzelechin-7-O-β-D-glucopyranoside (1), has beenisolated from the stem of Daphniphyllum oldhami.The structure of the new compound waselucidated on the basis of detailed spectroscopic analysis and comparison with related compounds.
A New Benzophenone from Securidaca inappendiculata
Xue Dong YANG , Li Zhen XU , Shi Lin YANG
2003, 14(9): 930-931
[Abstract](165) [FullText HTML] [PDF 706KB](0)
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A new benzophenone, securiphenone A was isolated from the roots of Securidaca inappendiculata.Its structure was determined as 2, 3-methylenedioxy-4-methoxybenzophenoneby spectroscopic methods.
A New Iridoid Glycoside and a New Iridoid from Pedicularis kansuensis f.aibiflora
Cheng Shan YUAN , Wei Dong XIE , Xiu Ping YANG , Zhong Jian JIA
2003, 14(9): 932-933
[Abstract](162) [FullText HTML] [PDF 755KB](1)
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A new iridoid glycoside 1 and a new iridoid 2 were isolated from the whole plant of Pedicularis kansuensis f.albiflora.Their structures were elucidated by spectroscopic methods.
A New Cyclic Peptide from Schnabelia tetradonta
Hui DOU , Yan ZHOU , Shu lin PENG , Li Sheng DING
2003, 14(9): 934-935
[Abstract](173) [FullText HTML] [PDF 785KB](2)
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A new cyclic octapeptide (schnabepeptide B) was isolated from the aerial part of Schnabelia tetradonta (Sun) C.Y.Wu et C.Chen (Lamiaceae).Its structure was elucidated as cyclo-(NH-Trp-Gly1-Leu1-Gly2-Pro1-Pro2-Leu2-Pro3-CO) on the basis of extensive 2D NMR andMS spectra.
A New Iridoid Glucoside from Lagotis yunnanensis
Xiao Dong YANG , Shuang Xi MEI , Jing Feng ZHAO , Gan Peng LI , Hong Bin ZHANG , Liang LI
2003, 14(9): 936-938
[Abstract](168) [FullText HTML] [PDF 860KB](0)
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Phytochemical investigation of Lagotis yunnanensis led to the isolation and identification of a new iridoid glucoside 1, named as 10-O-(3, 4-dimethoxy-(E)-cinnamoyl)aucubin.Its structure was elucidated by spectroscopic methods.
Two New Bromophenols from Red Alga Rhodomela confervoides
Xiao FAN , Nian Jun XU , Jian Gong SHI
2003, 14(9): 939-941
[Abstract](180) [FullText HTML] [PDF 1138KB](0)
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Two new bromophenols were isolated from Rhodomela confervoides.Their structrues were elucidated as 2, 2', 3-tribromo-3', 4, 4', 5-tetrahydroxy-6'-hydroxymethyldiphenylmethane and 2, 2', 3-tribromo-3', 4, 4', 5-tetrahydroxy-6'-ethyloxymethyldiphenylmethane by spectroscopic methods including IR, HREIMS, 1D and 2D NMR techniques.
Application of High Performance Liquid Chromatography to Separation of Novel Chiral Tetrahedral Heterometal Clusters
Xin Yi ZHU , Wei Qiang ZHANG , Yu Hua ZHANG , Li Ren CHEN , Yong Min LI
2003, 14(9): 942-945
[Abstract](166) [FullText HTML] [PDF 1347KB](0)
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A series of novel chiral tetrahedral heterometal clusters have firstly been separated oncellulose tris-(3,5-dimethylphenylcarbamate) stationary phase by high performance liquid chrom-atography, using hexane as the mobile phase with various alcohols as modifiers.
Separation of Phenolic Compounds and Organic Anions Using ODS Column Coated with Meso-octamethylcalix[4]pyrrole and Water as Eluent
Li Jun HE , Shi Jun SHAO , Yong GUO , Hua Jiao MA , Xia LIU , Sheng Xiang JIANG
2003, 14(9): 946-947
[Abstract](161) [FullText HTML] [PDF 876KB](0)
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Octadecylsilanized silica (ODS) was coated with meso-octamethylcalix[4]pyrrole to obtain a novel calix[4]pyrrole containing stationary phase for HPLC.Compared to ODS, the new stationary phase showed a relatively large retention and an improved separation for phenolic compounds and organic anions, using pure water as mobile phase.The results can be ascribed to the interaction between analytes and calix[4]pyrrole.
Size Dependence of First-order Hyperpolarizability of CdS Nanoparticles Studied by Hyper-Rayleigh Scattering
Yu ZHANG , Xin WANG , Ming MA , De Gang FU , Ning GU , Ju Zheng LIU , Zu Hong LU , Ling XU , Jun XU , Kun Ji CHEN
2003, 14(9): 948-951
[Abstract](170) [FullText HTML] [PDF 1882KB](0)
Abstract:
The second-order optical nonlinearity of CdS nanoparticles with different diameters of 28.0, 30.0, 31.5, 50.0, and 91.0 Å was studied by hyper-Rayleigh scattering technique.Results show that the first-order hyperpolarizability β value per CdS particle decreases as size is reduced to diameter of 31.5 Å; however, as CdS size further decreases, this trend is reversed and β value increases.Substantially, the normalized β value per CdS formula unit, β0, exhibits systematic enhancement with decreasing size.This phenomenon is interpreted in terms of a so-called surface contribution mechanism.
Determination of Amino Acids in an Individual Erythrocyteby Capillary Electrophoresis with Intracellular FITC-derivatization and Laser-induced Fluorescence Detection
Hua ZHANG , Wen Rui JIN
2003, 14(9): 952-954
[Abstract](159) [FullText HTML] [PDF 890KB](0)
Abstract:
A novel approach for analysis of amino acids in individual erythrocytes was established.In this method, the derivatization reagent was introduced into the living cells by electroporation.After derivatization, the amino acids in a single cell were determined by capillary electrophoresiswith laser-induced fluorescence detection.
Corrosion Inhibition of a Green Scale Inhibitor Polyepoxysuccinic Acid
Rong Chun XIONG , Qing ZHOU , Gang WEI
2003, 14(9): 955-957
[Abstract](171) [FullText HTML] [PDF 1251KB](5)
Abstract:
The corrosion inhibition of a green scale inhibitor, polyepoxysuccinic acid (PESA) was studied based on dynamic tests.It is found that when PESA is used alone, it had good corrosion inhibition.So, PESA should be included in the category of corrosion inhibitors.It is not only a kind of green scale inhibitor, but also a green corrosion inhibitor.The synergistic effect between PESA and Zn2+ or sodium gluconate is poor.However, the synergistic effect among PESA, Zn2+ and sodium gluconate is excellent, and the corrosion inhibition efficiency for carbon steel is higher than 99%.Further study of corrosion inhibition mechanism reveals that corrosion inhibition of PESA is not affected by carboxyl group, but by the oxygen atom inserted The existence of oxygen atom in PESA molecular structure makes it easy to form stable chelate with pentacyclic structure.
Dimerization of Propylene by Nickel (Ⅱ) and Cobalt (Ⅱ) Catalysts Based on Bidentate Nitrogen-phosphino Chelating Ligands
Si Zhong WU , Shi Wei LU
2003, 14(9): 958-961
[Abstract](146) [FullText HTML] [PDF 1732KB](1)
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The catalytic property of propylene dimerization by several nickel (Ⅱ), cobalt (Ⅱ) complexes containing N-P bidentate ligands was studied in combination with organoaluminum co-catalysts.The effects of the type of aluminum co-catalysts and its relative amount, the nature of precursors in terms of ligand backbone and metal center were investigated.The results indicated that precursor I (N,N-dimethyl-2-(diphenylphosphino) aniline nickel (Ⅱ) dichloride)exhibited high activity in propylene dimerization in the presence of the strong Lewis acid Et3Al2Cl3,whereas low productivity by its cobalt analogues was observed under identical reaction conditions.
The Role of Triplet State of Oligophenylenevinylenes (OPVs) in their Photooxidative Degradation
Li Chuan MA , Su Ping QIAN , Zhen Hui HAN , Xue Song WANG , Si De YAO , Jing Rong CHEN , Bo Jie WANG , Bao Wen ZHANG , Yi CAO
2003, 14(9): 962-965
[Abstract](139) [FullText HTML] [PDF 1624KB](0)
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Results of triplet-triplet energy transfer from biacetyl to OPVs and OPV triplet state quenching by 1, 4-diazabicyclo[2.2.2] octane (DABCO) suggested that triplet state of oligophenylenevinylenes(OPVs) directly takes part in their photooxidative degradation instead of just generating singlet oxygen.
The Solvent Effect on the Chemoselectivity of Palladium-catalyzed Oligomerization of 3, 3-Dimethyl-1-butyne
Jin Sheng CHENG , Jin Heng LI , Huan Feng JIANG , Xiao Yue OUYANGLCLC
2003, 14(9): 966-968
[Abstract](137) [FullText HTML] [PDF 1134KB](0)
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The chemoselectivities of PdCl2 and CuCl2-catalyzed oligomerization of 3, 3-dimethyl-butyne:1, 3, 5-tri-tert-butylbenzene, 2, 2, 7, 7-tetramethyl-3, 6-dichloro-3, 5-octadiene and 2, 2, 7,7- tetramethyl-3,5-octadiyne were obtained, respectively, by regulating the polarity of the solvent.
Controlling Pore Size and its Distribution of γ-Al2O3 Nanofiltration Membranes
Rong Chun XIONG , Xiao Dong LEI , Gang WEI
2003, 14(9): 969-972
[Abstract](146) [FullText HTML] [PDF 1402KB](0)
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The preparation process of γ-Al2O3 nanofiltration membranes were studied by N2 absorption and desorption test and retention rate vs thickness gradient curve method.It was found that template and thermal treatment were key factors for controlling pore size and its distribution.Under the optimized experimental conditions, the BJH (Barret-Joyner-Halenda) desorption average pore diameter, BJH desorption cumulative volume of pores and BET (Brunauer-Emmett-Teller) surface area of obtained membranes were about 3.9 nm, 0.33 cm3/g and 245 m2/g respectively, the pore size distribution was very narrow.Pore size decreased with the increasing of thickness and no evident change after the dense top layer was formed.The optimum thickness can be controlled by retention rate vs thickness gradient curve method.
Synthesis of LDHs and Rheological Properties of Laponite/LDHs Dispersions
Pei Zhi GUO , De Jun SUN , Jie ZHANG
2003, 14(9): 973-976
[Abstract](136) [FullText HTML] [PDF 1462KB](0)
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The chemical composition, morphology of the particles of positively charged layered double hydroxides (LDHs) were studied by ICP, Mastersizer, TEM.The preliminary results indicated that with adding LDHs to 1% laponite dispersion the yield stress oflaponite/LDHs mixed dispersions increased at first, then decreased dramatically to a minimum, and the yield stress rose again when LDHs increased further.
Size Effects of Nano-crystalline Cellulose
Guo Kang LI , Xiao Fang LI , Yong JIANG , Mei Zhen ZENG , En Yong DING
2003, 14(9): 977-978
[Abstract](153) [FullText HTML] [PDF 759KB](0)
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Natural cellulose with the crystal form of cellulose Ⅰ, when treated with condensed lye(e.g.18%NaOH), can change into new crystal form of cellulose Ⅱ.But the nano-crystallinecellulose(NCC) can do it when only treated with dilute lye (e.g.1%NaOH) at room temperatureand even can dissolve into slightly concentrated lye (e.g.4%NaOH).
Preparation and Selectivity of Molecularly Imprinted Polymer Coating on the Micro Pore Membrane of Polytetrafluoroethylene
Hong Sheng GUO , Yu Mei JIA , Xi Wen HE
2003, 14(9): 979-982
[Abstract](140) [FullText HTML] [PDF 1430KB](0)
Abstract:
In order to obtain mechanically stable membrane for practical application, the imprinted polymer was synthesized in the pores of polyfluoromembrane, the binding and transport ability of the membrane were studied.
Indirect Determination of Ascorbic Acid with Ammonium Sulfate and Isopropyl Alcohol by Extraction-flotation of Copper
Shao Mei WANG , Yun XING , Quan Min LI
2003, 14(9): 983-986
[Abstract](153) [FullText HTML] [PDF 1357KB](0)
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A new method of indirect determination of ascorbic acid(Vc) with ammonium sulfate and isopropyl alcohol by extraction-flotation of copper is studied in this paper.It shows that a small amount of Cu(Ⅱ) can be reduced to Cu(Ⅰ) by Vc, then Cu(Ⅰ) reacted with the SCN-,which precipitated on the interface of isopropyl alcohol and H2O.A good linear relationship is observed between the flotation yield(E) of Cu(Ⅱ) and the amount of Vc.The detection limit for Vc is 1.76μg/mL.The method is simple, rapid (5 min), but suffers from little interference of common anions and cations.It has been successfully applied for the determination of Vc in fruits.
Application of Genetic Programming in Predicting Infinite Dilution Activity Coefficients of Organic Compounds in Water
Yi Lin CAO , Huan Ying LI
2003, 14(9): 987-990
[Abstract](135) [FullText HTML] [PDF 1354KB](0)
Abstract:
In this paper, we calculated 37 structural descriptors of 174 organic compounds.The 154 molecules were used to derive quantitative structure-infinite dilution activity coefficient relationship by genetic programming, the other 20 compounds were used to test the model.The result showed that molecular partition property and three-dimensional structural descriptors have significant influence on the infinite dilution activity coefficients.
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