Protein tyrosine phosphatase 1B （PTP1B） plays an important role as a negative regulator and has been proved to be an effective target for the treatment of type 2 diabetes mellitus. Bis-（2,3-dibromo-4,5-dihydroxyphe...Protein tyrosine phosphatase 1B （PTP1B） plays an important role as a negative regulator and has been proved to be an effective target for the treatment of type 2 diabetes mellitus. Bis-（2,3-dibromo-4,5-dihydroxyphenyl）-methane 7 was first reported as a natural bromophenol with significant inhibition against PTP1B which was isolated from red algae Rhodomela conrervoides. Intrigued by its astonishing activity （IC50 = 2.4 μmol/L）, compound 7 was synthesized with the overall yield of 24% and evaluated for its PTPIB inhibitory activity compared with natural compound.展开更多
A simple, efficient, and environment benign route was developed for the preparation of bis-（indolyl）methanes and 14-aryl-14H- dibenzo[aj]xanthenes from condensation of various aromatic aldehydes or ketones with indo...A simple, efficient, and environment benign route was developed for the preparation of bis-（indolyl）methanes and 14-aryl-14H- dibenzo[aj]xanthenes from condensation of various aromatic aldehydes or ketones with indole, and 2-naphthol, respectively, using oxalic acid catalyst in aqueous medium. Use of cheap and easily available catalyst, better yields and simple reaction protocol are the advantages of the present method.展开更多
Studies on the degradation process of waste polyethylene terephthalate(PET)have become increasingly mature,but there are relatively few studies on the separation of degradation products.The products contain many compo...Studies on the degradation process of waste polyethylene terephthalate(PET)have become increasingly mature,but there are relatively few studies on the separation of degradation products.The products contain many components and the separation of which is difficult.Therefore,the study on phase equilibrium thermodynamics of bis-2-hydroxyethyl terephthalate(BHET)is of great theoretical significance and practical value to provide basic data for the BHET crystallization separation.In this work,the degraded products were purified and characterized.The solubility of BHET in methanol,ethanol,ethylene glycol,water and the mixture of ethylene glycol+water were determined by static method.The experimental results were correlated with different models,such as ideal solution(IS)model,λh equation,Apelblat equation and NRTL model.Based on the van’t Hoff equation,the mixing Gibbs energy,enthalpy and entropy were calculated.From this work,the basic data which can be used to guide the crystallization process of BHET were obtained,including solubility data,correlation model and thermodynamic properties.展开更多
Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as ...Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as the catalysts for the synthesis of bisdihydropyrimidin -2(1H)-ones from aromatic dialdehydes,1,3-dicarbonyl compounds and urea at 90℃under solvent-free conditions.展开更多
This work presents a new greener alternative for biocondensation of aldehydes and indoles for the synthesis of bis- and tris(indolyl)methanes catalyzed by lemon juice (Citrus limon) in good yields under ultrasound irr...This work presents a new greener alternative for biocondensation of aldehydes and indoles for the synthesis of bis- and tris(indolyl)methanes catalyzed by lemon juice (Citrus limon) in good yields under ultrasound irradiation in aqueous ethanol. Various substituted aldehydes with indoles under this reaction condition are elucidated. Also, tetraindolyl compounds were prepared using terephthaldialdehyde by following the same protocol. This method is an environmentally benign, efficient reaction, which requires shorter reaction time and simple experimental and work-up procedures.展开更多
The title compound bis-9-fluorenylmethylphenyl silane (C33H26Si, Mr = 450.63) was synthesized and its structure has been synthesized and determined by X-ray analysis. The crystal is of triclinic, space group P with a ...The title compound bis-9-fluorenylmethylphenyl silane (C33H26Si, Mr = 450.63) was synthesized and its structure has been synthesized and determined by X-ray analysis. The crystal is of triclinic, space group P with a = 9.478(1), b = 10.0956(1), c = 13.0243(2) ? a = 92.668(2), b = 90.809(2), g = 99.348(2)? l = 0.71073 ?, m(MoKa) = 0.115 mm-1, V = 1288.1(2) 3, Z = 2, Dc = 1.219 g/cm3 and F(000) = 476. The structure was refined to R = 0.0437 and wR(F2) = 0.0963 for 3346 observed reflections with I>2s(I). X-ray diffraction analysis reveals that the title compound is bis-9-fluorenylmethylphenyl silane.展开更多
The title compound 1 was synthesized from 1.2:5,6-dianhydro-3,4-dianhydro-3,4-isopropylideneD-mannitol 2 through four steps in a total yield of 53%. The absolute configuration of this compound was confirmed by X-ray d...The title compound 1 was synthesized from 1.2:5,6-dianhydro-3,4-dianhydro-3,4-isopropylideneD-mannitol 2 through four steps in a total yield of 53%. The absolute configuration of this compound was confirmed by X-ray diffraction.展开更多
The new ligand bis-（1,4-sodium thiolactate） butane （L）-O2CCH3S-（CH2）4SCHCH3CO2- has been prepared from the reaction of disodium salt of thiolactic acid and 1,4-dichlorobutane, while the disodium thiolactate was ...The new ligand bis-（1,4-sodium thiolactate） butane （L）-O2CCH3S-（CH2）4SCHCH3CO2- has been prepared from the reaction of disodium salt of thiolactic acid and 1,4-dichlorobutane, while the disodium thiolactate was prepared instanteously through the reaction of thiolactic acid with NaOH. Mono and dinuclear complexes were obtained by direct reaction of the above ligands with H[AuCI4] in 1 ： 1, 2：1, 1：2, 2：2 and 3：1 ligands to metal molar ratio. The prepared complexes were characterized by elemental analysis, spectral studies FTIR （Fourier transform Infrared） and UV-Vis, magnetic measurement, conductivity measurement and IHNMR for the ligand （L） and some of the complexes. The conductance data indicate that the complexes of the formulas Na[Au（SCH3CHCOO）2], Na[Au（SCH3CHCOO）（OOCCHCH3SH）2] and [Au（L）]Cl are 1：1 electrolyte. Electronic spectra and magnetic moment values indicate the presence of square planner geometry around Au（III） ions.展开更多
Smooth and strong copper foils are highly required for the development of printed circuit boards and Li-ion batteries.Adding additives is an efficient and low-cost method to enhance electrodeposited copper foils.Here ...Smooth and strong copper foils are highly required for the development of printed circuit boards and Li-ion batteries.Adding additives is an efficient and low-cost method to enhance electrodeposited copper foils.Here we chose Bis-(3-sulfopropyl)-disulfide(SPS)as the additive and investigated its concentration on the surface roughness and tensile strength of the electrodeposited copper foils.A copper foil with the smoothest surface(Rz=2.1μm)and the highest tensile strength(~338 MPa)was prepared with1.5 mg/L SPS.The contact angle on the copper foil decreased with the reduction of surface roughness.The enhancing mechanism of the SPS was investigated by scanning electron microscopy and X-ray diffraction.The refined grain and enhanced(220)texture were considered to be the radical reason for the smooth and strong copper foils.The electrochemical results prove the suppressing effect is related to the SPS adsorption.展开更多
The geometric conformation and electronic structure of bis-（5-nitro-2H-tetrazolato-N2）tetraammine cobalt（Ⅲ） perchlorate and its Ni/Fe/Cu/Zn analogues are studied under the TPSS （Tao-Perdew-Staroverov-Scuseria） ...The geometric conformation and electronic structure of bis-（5-nitro-2H-tetrazolato-N2）tetraammine cobalt（Ⅲ） perchlorate and its Ni/Fe/Cu/Zn analogues are studied under the TPSS （Tao-Perdew-Staroverov-Scuseria） levels of density functional theory in order to throw light on the relationship between their energy gaps and impact sensitivity While the perchlorate ions are coordinated with the copper cation, which is different from the other four compounds NBO （Natural bond orbital） analyses indicated that the metal-ligand interaction in the Co complex is covalent, while the others are ionic. The analysis of the electrostatic potential demonstrated that the O atoms from the nitro-tetrazole ring and perchlorate were primarily negative, while the other atoms were positive. The study was also conducted to gain a better understanding of the correlation of the energy gap and impact sensitivity.展开更多
The series of salen-bridged bis-pillar[1]arenes were conveniently prepared by condensation reaction of5,5'-methylenebis(2-hydroxybenzalde hyde)or 5,5'-(propane-2,2-diyl)bis(2-hydroxybenzaldehyde)with mono-amid...The series of salen-bridged bis-pillar[1]arenes were conveniently prepared by condensation reaction of5,5'-methylenebis(2-hydroxybenzalde hyde)or 5,5'-(propane-2,2-diyl)bis(2-hydroxybenzaldehyde)with mono-amido-functionalized pillar[5]arenes containing different terminal aminoalkyl groups in refluxing ethanol.The^1H NMR and 2D-NOESY spectra indicated that the salen-bridged bis-pillar[5]arenes with longer allcylene linker(n=3,4,6)formed the fascinating bis-[1]rotaxanes,while the salenbridged bis-pillar[5]arenes with short hydrazine and ethylenediamino linker(n=0,2)predominately existed in free form.The single crystal structure of the bis-pillar[5]are ne ambiguously indicated that two propylenediamino linker inserted in to two cavities of pillar[5]arene to form a novel bis-[1]rotaxanes.展开更多
Herein, we reported the synthesis and investigation of highly luminescent quadruple-stranded helicate （C6H 16N）4[Eu2（MBDA）4]2·3 C4H10O.4C2H 3N（ 1-Eu） [H2M B DA=N-methyl-4,4＇-b i s（4,4,4-tri fl uoro-1,3-di...Herein, we reported the synthesis and investigation of highly luminescent quadruple-stranded helicate （C6H 16N）4[Eu2（MBDA）4]2·3 C4H10O.4C2H 3N（ 1-Eu） [H2M B DA=N-methyl-4,4＇-b i s（4,4,4-tri fl uoro-1,3-dioxob utyl）di- phenylamine] for its stability toward metal ions in the solution. The material was characterized via X-ray crystallo- graphic technique, Fourier transform infrared（FTIR） spectroscopy and electrospray ionization quadrapole time-of- flight（ESI-TOF） mass spectrometry. The results on the luminescence quantum yields clearly demonstrate that the ligand can effectively sensitize the luminescence of the Eu3＋ ions（φoverall=15%）. Upon the addition of different metal ions（i, e., Ag＋, Cd2＋, Zn2＋, Fe3＋, A13＋ and Ni2＋） to the CH3CN solution of compound I-Eu, the emission intensities of Eu3＋ ions at 612 nm were affected to some extent, which could be attributed to the presence of ion exchanges between Eu3＋ ions and the metals ions, and the result was confirmed by ESI-TOF mass spectrometry.展开更多
Two strategies for the design of new pillar[5]arene-based mechanically self-interlocked molecules (MSMs) are reported here. The first strategy is based on the construction of an intermediate pseudo[1]rotaxane followed...Two strategies for the design of new pillar[5]arene-based mechanically self-interlocked molecules (MSMs) are reported here. The first strategy is based on the construction of an intermediate pseudo[1]rotaxane followed by the desired bis-[l]rotaxane. The other one is based on the construction of the desired bis-[1]rotaxane directly via a condensation reaction through host-guest interactions between a mono-functionalized pillar[5]arene and the axle. The newly synthesized bis-[1]rotaxane BR was characterized by ~1H NMR, ^(13)C NMR, 2D NMRs (~1H-^(13)C HSQC,~1H-~1H COSY and NOESY) and LC-ESI-MS,which indicated compound BR displayed an self-interlocked structure in CDCl_3. Surprisingly, the results of SEM, TEM and DLS showed that the compound BR could assemble into spherical nanoparticles in MeOH.展开更多
A series of（Z）-2-chloro-1,3-diarylpropen-1-ones were unexpectedly synthesized in moderate yields by treatment of easily available 2,3-epoxy-1,3-diarylpropan-1-ones with Vilsmeier reagent,which was derived from bis（...A series of（Z）-2-chloro-1,3-diarylpropen-1-ones were unexpectedly synthesized in moderate yields by treatment of easily available 2,3-epoxy-1,3-diarylpropan-1-ones with Vilsmeier reagent,which was derived from bis（trichloromethyl） carbonate（BTC, triphosgene） and DMF.A possible mechanism was also proposed,where sequential ring-opening,halogenation and elimination reactions were involved.展开更多
A series of new chiral 2（5H）-furanone derivatives containing bis-l,2,3-triazole moiety were designed and syn- thesized from （5S）-5-alkoxy-3,4-dihalo-2（5H）-furanones 1, dicarboxyl amino acids 2, propargyl bromide...A series of new chiral 2（5H）-furanone derivatives containing bis-l,2,3-triazole moiety were designed and syn- thesized from （5S）-5-alkoxy-3,4-dihalo-2（5H）-furanones 1, dicarboxyl amino acids 2, propargyl bromide, and or- ganic azides 5 under mild conditions via the sequential three steps, including asymmetric Michael addi- tion-elimination, substitution and no-ligand click reaction. Twelve new intermediates, including N-[5-alkoxy- 2（5H）-furanonyl] dicarboxyl amino acids 3 and their corresponding propargyl esters 4, and twelve target molecules 6 were characterized by FTIR, 1H NMR, 13C NMR, MS and elemental analysis. The influences of different syn- thetic conditions and substrates in each step were investigated. The research provides a new method and idea for the synthesis of 2（5H）-furanone compounds with polyheterocyclic structure due to the diversities of four basic unit molecules.展开更多
Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). Th...Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.展开更多
基金the National Center for Drug Screening (Shanghai,PR China) for supplying data on PTP1B inhibitory activities of compoundssupported by the National 863 projects (Nos.2007AA09Z410 and 2007AA091604).
文摘Protein tyrosine phosphatase 1B （PTP1B） plays an important role as a negative regulator and has been proved to be an effective target for the treatment of type 2 diabetes mellitus. Bis-（2,3-dibromo-4,5-dihydroxyphenyl）-methane 7 was first reported as a natural bromophenol with significant inhibition against PTP1B which was isolated from red algae Rhodomela conrervoides. Intrigued by its astonishing activity （IC50 = 2.4 μmol/L）, compound 7 was synthesized with the overall yield of 24% and evaluated for its PTPIB inhibitory activity compared with natural compound.
文摘A simple, efficient, and environment benign route was developed for the preparation of bis-（indolyl）methanes and 14-aryl-14H- dibenzo[aj]xanthenes from condensation of various aromatic aldehydes or ketones with indole, and 2-naphthol, respectively, using oxalic acid catalyst in aqueous medium. Use of cheap and easily available catalyst, better yields and simple reaction protocol are the advantages of the present method.
基金financially supported by the National Key Research and Development Program of China(2019YFC1908204)the National Natural Scientific Fund of China(No.21878292,21776289,21908232,21978291)+1 种基金Innovation Academy forGreen Manufacture,Chinese Academy of Sciences(No.IAGM2020C12,IAGM2020C21 and IAGM-2019-A06)K.C.Wong Education Foundation(No.GJTD-2018-04)。
文摘Studies on the degradation process of waste polyethylene terephthalate(PET)have become increasingly mature,but there are relatively few studies on the separation of degradation products.The products contain many components and the separation of which is difficult.Therefore,the study on phase equilibrium thermodynamics of bis-2-hydroxyethyl terephthalate(BHET)is of great theoretical significance and practical value to provide basic data for the BHET crystallization separation.In this work,the degraded products were purified and characterized.The solubility of BHET in methanol,ethanol,ethylene glycol,water and the mixture of ethylene glycol+water were determined by static method.The experimental results were correlated with different models,such as ideal solution(IS)model,λh equation,Apelblat equation and NRTL model.Based on the van’t Hoff equation,the mixing Gibbs energy,enthalpy and entropy were calculated.From this work,the basic data which can be used to guide the crystallization process of BHET were obtained,including solubility data,correlation model and thermodynamic properties.
文摘Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as the catalysts for the synthesis of bisdihydropyrimidin -2(1H)-ones from aromatic dialdehydes,1,3-dicarbonyl compounds and urea at 90℃under solvent-free conditions.
文摘This work presents a new greener alternative for biocondensation of aldehydes and indoles for the synthesis of bis- and tris(indolyl)methanes catalyzed by lemon juice (Citrus limon) in good yields under ultrasound irradiation in aqueous ethanol. Various substituted aldehydes with indoles under this reaction condition are elucidated. Also, tetraindolyl compounds were prepared using terephthaldialdehyde by following the same protocol. This method is an environmentally benign, efficient reaction, which requires shorter reaction time and simple experimental and work-up procedures.
文摘The title compound bis-9-fluorenylmethylphenyl silane (C33H26Si, Mr = 450.63) was synthesized and its structure has been synthesized and determined by X-ray analysis. The crystal is of triclinic, space group P with a = 9.478(1), b = 10.0956(1), c = 13.0243(2) ? a = 92.668(2), b = 90.809(2), g = 99.348(2)? l = 0.71073 ?, m(MoKa) = 0.115 mm-1, V = 1288.1(2) 3, Z = 2, Dc = 1.219 g/cm3 and F(000) = 476. The structure was refined to R = 0.0437 and wR(F2) = 0.0963 for 3346 observed reflections with I>2s(I). X-ray diffraction analysis reveals that the title compound is bis-9-fluorenylmethylphenyl silane.
文摘The title compound 1 was synthesized from 1.2:5,6-dianhydro-3,4-dianhydro-3,4-isopropylideneD-mannitol 2 through four steps in a total yield of 53%. The absolute configuration of this compound was confirmed by X-ray diffraction.
文摘The new ligand bis-（1,4-sodium thiolactate） butane （L）-O2CCH3S-（CH2）4SCHCH3CO2- has been prepared from the reaction of disodium salt of thiolactic acid and 1,4-dichlorobutane, while the disodium thiolactate was prepared instanteously through the reaction of thiolactic acid with NaOH. Mono and dinuclear complexes were obtained by direct reaction of the above ligands with H[AuCI4] in 1 ： 1, 2：1, 1：2, 2：2 and 3：1 ligands to metal molar ratio. The prepared complexes were characterized by elemental analysis, spectral studies FTIR （Fourier transform Infrared） and UV-Vis, magnetic measurement, conductivity measurement and IHNMR for the ligand （L） and some of the complexes. The conductance data indicate that the complexes of the formulas Na[Au（SCH3CHCOO）2], Na[Au（SCH3CHCOO）（OOCCHCH3SH）2] and [Au（L）]Cl are 1：1 electrolyte. Electronic spectra and magnetic moment values indicate the presence of square planner geometry around Au（III） ions.
基金the National Key R&D Program of China(No.2017YFB1200800)the National Natural Science Foundation of China(Nos.51827810 and 51637009)the Fundamental Research Funds for the Central Universities(2018XZZX001-05)。
文摘Smooth and strong copper foils are highly required for the development of printed circuit boards and Li-ion batteries.Adding additives is an efficient and low-cost method to enhance electrodeposited copper foils.Here we chose Bis-(3-sulfopropyl)-disulfide(SPS)as the additive and investigated its concentration on the surface roughness and tensile strength of the electrodeposited copper foils.A copper foil with the smoothest surface(Rz=2.1μm)and the highest tensile strength(~338 MPa)was prepared with1.5 mg/L SPS.The contact angle on the copper foil decreased with the reduction of surface roughness.The enhancing mechanism of the SPS was investigated by scanning electron microscopy and X-ray diffraction.The refined grain and enhanced(220)texture were considered to be the radical reason for the smooth and strong copper foils.The electrochemical results prove the suppressing effect is related to the SPS adsorption.
基金Supporting information for this article is available on the WWW under http：//dx.doi.org/10.1002/cjoc.201280027 or from the author. Acknowledgment We gratefully acknowledge the financial support from the National Natural Science Foundation of China （No. 10776002） and China Academy of Engineering Physics （No. 20911120033）, the project of State Key Laboratory of Science and Technology （Nos. QNKT11-06, YBKT10-03）, and the Program for New Centu17 Excellent Talents in University （No. NCET-09-005I）. Our thanks are due to Professor Gustavo E. Scuseria for providing the development version of Gaussian program.
文摘The geometric conformation and electronic structure of bis-（5-nitro-2H-tetrazolato-N2）tetraammine cobalt（Ⅲ） perchlorate and its Ni/Fe/Cu/Zn analogues are studied under the TPSS （Tao-Perdew-Staroverov-Scuseria） levels of density functional theory in order to throw light on the relationship between their energy gaps and impact sensitivity While the perchlorate ions are coordinated with the copper cation, which is different from the other four compounds NBO （Natural bond orbital） analyses indicated that the metal-ligand interaction in the Co complex is covalent, while the others are ionic. The analysis of the electrostatic potential demonstrated that the O atoms from the nitro-tetrazole ring and perchlorate were primarily negative, while the other atoms were positive. The study was also conducted to gain a better understanding of the correlation of the energy gap and impact sensitivity.
基金financial support by the National Natural Science Foundation of China(Nos.21372192,21871227)the Priority Academic Program Development of Jiangsu Higher Education Institutions。
文摘The series of salen-bridged bis-pillar[1]arenes were conveniently prepared by condensation reaction of5,5'-methylenebis(2-hydroxybenzalde hyde)or 5,5'-(propane-2,2-diyl)bis(2-hydroxybenzaldehyde)with mono-amido-functionalized pillar[5]arenes containing different terminal aminoalkyl groups in refluxing ethanol.The^1H NMR and 2D-NOESY spectra indicated that the salen-bridged bis-pillar[5]arenes with longer allcylene linker(n=3,4,6)formed the fascinating bis-[1]rotaxanes,while the salenbridged bis-pillar[5]arenes with short hydrazine and ethylenediamino linker(n=0,2)predominately existed in free form.The single crystal structure of the bis-pillar[5]are ne ambiguously indicated that two propylenediamino linker inserted in to two cavities of pillar[5]arene to form a novel bis-[1]rotaxanes.
基金Supported by the National Natural Science Foundation of China（Nos.21572048, 21102039, 21272061, 51302068） and the Open Project of the State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, China.
文摘Herein, we reported the synthesis and investigation of highly luminescent quadruple-stranded helicate （C6H 16N）4[Eu2（MBDA）4]2·3 C4H10O.4C2H 3N（ 1-Eu） [H2M B DA=N-methyl-4,4＇-b i s（4,4,4-tri fl uoro-1,3-dioxob utyl）di- phenylamine] for its stability toward metal ions in the solution. The material was characterized via X-ray crystallo- graphic technique, Fourier transform infrared（FTIR） spectroscopy and electrospray ionization quadrapole time-of- flight（ESI-TOF） mass spectrometry. The results on the luminescence quantum yields clearly demonstrate that the ligand can effectively sensitize the luminescence of the Eu3＋ ions（φoverall=15%）. Upon the addition of different metal ions（i, e., Ag＋, Cd2＋, Zn2＋, Fe3＋, A13＋ and Ni2＋） to the CH3CN solution of compound I-Eu, the emission intensities of Eu3＋ ions at 612 nm were affected to some extent, which could be attributed to the presence of ion exchanges between Eu3＋ ions and the metals ions, and the result was confirmed by ESI-TOF mass spectrometry.
文摘Two strategies for the design of new pillar[5]arene-based mechanically self-interlocked molecules (MSMs) are reported here. The first strategy is based on the construction of an intermediate pseudo[1]rotaxane followed by the desired bis-[l]rotaxane. The other one is based on the construction of the desired bis-[1]rotaxane directly via a condensation reaction through host-guest interactions between a mono-functionalized pillar[5]arene and the axle. The newly synthesized bis-[1]rotaxane BR was characterized by ~1H NMR, ^(13)C NMR, 2D NMRs (~1H-^(13)C HSQC,~1H-~1H COSY and NOESY) and LC-ESI-MS,which indicated compound BR displayed an self-interlocked structure in CDCl_3. Surprisingly, the results of SEM, TEM and DLS showed that the compound BR could assemble into spherical nanoparticles in MeOH.
基金the National Natural Science Foundation of China(Nos.20806073 and 20876147)the National Key Technology Research and Development Program(No.2007BAI34B06) for financial support
文摘A series of（Z）-2-chloro-1,3-diarylpropen-1-ones were unexpectedly synthesized in moderate yields by treatment of easily available 2,3-epoxy-1,3-diarylpropan-1-ones with Vilsmeier reagent,which was derived from bis（trichloromethyl） carbonate（BTC, triphosgene） and DMF.A possible mechanism was also proposed,where sequential ring-opening,halogenation and elimination reactions were involved.
基金We are grateful to the National Natural Science Foundation of China （No. 20772035）, the Third Talents Special Funds of Guangdong Higher Education （No. Guangdong-Finance-Education [2011]431） and the Natural Science Foundation of Guangdong Province （No. S2011010001556） for financial support.
文摘A series of new chiral 2（5H）-furanone derivatives containing bis-l,2,3-triazole moiety were designed and syn- thesized from （5S）-5-alkoxy-3,4-dihalo-2（5H）-furanones 1, dicarboxyl amino acids 2, propargyl bromide, and or- ganic azides 5 under mild conditions via the sequential three steps, including asymmetric Michael addi- tion-elimination, substitution and no-ligand click reaction. Twelve new intermediates, including N-[5-alkoxy- 2（5H）-furanonyl] dicarboxyl amino acids 3 and their corresponding propargyl esters 4, and twelve target molecules 6 were characterized by FTIR, 1H NMR, 13C NMR, MS and elemental analysis. The influences of different syn- thetic conditions and substrates in each step were investigated. The research provides a new method and idea for the synthesis of 2（5H）-furanone compounds with polyheterocyclic structure due to the diversities of four basic unit molecules.
文摘Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.
