Two new organic supramolecular cocrystal complexes C18H18O4·C10H8N2（I） and C18H18O4·C12H10N2（II）（C18H18O4 = 2,3,6,7-tetrahydroxyl-9,10-dimethyl-9,10-dihydro-9,10-ethanoanthracene（LH4）, C10H8N2 = 4,4＇...Two new organic supramolecular cocrystal complexes C18H18O4·C10H8N2（I） and C18H18O4·C12H10N2（II）（C18H18O4 = 2,3,6,7-tetrahydroxyl-9,10-dimethyl-9,10-dihydro-9,10-ethanoanthracene（LH4）, C10H8N2 = 4,4＇-bipyridine（bpy） and C12H10N2 = 4,4＇-bipyridinylethane（bpe）） have been obtained by mixing LH4 with corresponding bpy or bpe ligand. The two complexes have been determined by X-ray crystal structure analysis, elemental analysis and IR analysis. Compound I crystallizes in the orthorhombic Pnma with a = 9.7078（4）, b = 22.4974（10）, c = 20.6272（9） V = 4505.0（3）3, Mr = 454.51, Dc. = 1.340 g·cm^-3, μ = 0.09 mm-1, F（000） = 1920, Z = 8, R = 0.0503 and wR = 0.1360. Compound II crystallizes in monoclinic C2/c with a = 29.944（6）, b = 9.820（2）, c = 22.643（5） , V = 5048.4（18）3, Mr = 480.54, Dc. = 1.265 g cm^–3, μ = 0.084 mm^–1, F（000） = 2032, Z = 8, R = 0.0548 and wR = 0.1600. X-ray single-crystal structure analysis shows that two-dimensional（2D） layer supramolecular structures are formed through hydrogen bonds and π-π interactions in the two complexes. IR analysis also indicates that there are only associated hydroxyl groups in the two complexes.展开更多
A new environmental friendly catalyst, HaSiWrMo6O40/PAn was prepared and identified by means of FT-IR, XRD and TG/DTA. The optimum conditions have been found, that was, mass ratio of m（PAn）： m（HaSiW6Mo6On.） was 1...A new environmental friendly catalyst, HaSiWrMo6O40/PAn was prepared and identified by means of FT-IR, XRD and TG/DTA. The optimum conditions have been found, that was, mass ratio of m（PAn）： m（HaSiW6Mo6On.） was 1：1.25, volume of methanol was 20 mL, and the reflux reaction time was 2h. The structural identity of Keggin units was preserved after the incorporation into polyaniline matrix. H4SiW6Mo6040/PAn was used as catalyst in catalytic synthesis of acetals and ketals. Effects of n（aldehyde（ketone ））： n（glycol）, catalyst dosage and reaction time on yield were investingated. Optimal conditions were： n（aldehyde（ketone））： n（glycol）=1.0： 1.5; mass fraction of catalyst to reactants, 0.5%; reaction time, 1.0 h and cyclohexane as water-stripped reagent, 15 mL. Under these conditions, yields of actels and ketals were 31.9%-91.6%.展开更多
A new method has been developed for separation and determination of zinc,copper,cobalt and nickel based on their colour chelates with 6,6″-dimethyl-4′-phenyl-2,2′:6′,2″-terpyridine（TPY） by ion pair high perform...A new method has been developed for separation and determination of zinc,copper,cobalt and nickel based on their colour chelates with 6,6″-dimethyl-4′-phenyl-2,2′:6′,2″-terpyridine（TPY） by ion pair high performance liquid chromatography in a reversed phase mode.The suitable conditions are the methanol-water（80:20,V/V） containing 10mmol/L NaH2PO4-H3PO4 buffer solution（pH=5.0） and 3.0mmol/L sodium dodecyl sulfonate as mobile phase,on a Symmetry C18 column（3.9mmID×150mm）,the flow rate of the mobile phase is 1.0mL/min.Spectrophotometric detection was made at 340nm.The detective limits are 0.05,0.10,2.00 and 0.50ng/mL respectively.The method has good selectivity and sensitivity.It has been applied to the separation and determination of zinc,copper,cobalt and nickel in human hair and tobacco and the result is satisfied.展开更多
The title compound (p-methylphenylbis(4, 4-dimethyl-6-hydroxycyclohexene-1-one-2-yl)methane) has been synthesized by the reaction of 4-methylbenzaldehyde and 5, 5-dimethyl-1, 3-cyclohexanedione in N,N-dimethylformamid...The title compound (p-methylphenylbis(4, 4-dimethyl-6-hydroxycyclohexene-1-one-2-yl)methane) has been synthesized by the reaction of 4-methylbenzaldehyde and 5, 5-dimethyl-1, 3-cyclohexanedione in N,N-dimethylformamide. Its structure was determined by single crystal X-ray diffraction. The Crystal is monoclinic, space group P21/a, a=0. 9304 (2)nm, b=1. 1754 (2)nm, c=2. 0134 (4)nm, β=102. 40(2)°, Mr= 382. 50, V=2. 1505 (7)nm3, Dc = 1. 181g/cm3, Z=4, μ(MoKα) = 0. 79cm-1, F(000) = 856.The structure was solved by direct methods, and refined by full-matris least-Squares method to a final R =0. 042 and Rw = 0. 045. The crystal structure shows that there are two conjugated enol form in the molecule.展开更多
Objective:To isolate and characterize the cytotoxic compounds from Diospyros quercina(Baill.)G.E.Schatz&Lowry(Ebenaceae).Methods:An ethno-botanical survey was conducted in the south of Madagascar from July to Augu...Objective:To isolate and characterize the cytotoxic compounds from Diospyros quercina(Baill.)G.E.Schatz&Lowry(Ebenaceae).Methods:An ethno-botanical survey was conducted in the south of Madagascar from July to August 2010.Bio-guided fractionation assay was carried out on the root bark of Diospyros quercina,using cytotoxicity bioassay on murine P388 leukemia cell lines as model.The structures of the cytotoxic compounds were elucidated by 1D and 2D NMR spectroscopy and mass spectrometry.Results:Biological experiments resulted in the isolation of three bioactive pure compounds(named TR-21,TR-22,and TR-23)which exhibited very good in vitro cytotoxic activities with the IC_(50)values of(0.017 5±0.0060)μg/mL,(0.089±0.005)μg/mL and(1.027±0.070)μg/mL respectively.Thus,they support the claims of traditional healers and suggest the possible correlation between the chemical composition of this plant and its wide use in Malagasy folk medicine to treat cancer.Conclusions:The ability of isolated compounds in this study to inhibit cell growth may represent a rational explanation for the use of Diospyros quercina root bark in treating cancer by Malagasy traditional healers.Further studies are,therefore,necessary to evaluate the in vivo antineoplastic activity of these cytotoxic compounds as effective anticancer drugs.展开更多
基金supported by the National Natural Science Foundation of China(No.21176246)Jiangsu Qinglan Project
文摘Two new organic supramolecular cocrystal complexes C18H18O4·C10H8N2（I） and C18H18O4·C12H10N2（II）（C18H18O4 = 2,3,6,7-tetrahydroxyl-9,10-dimethyl-9,10-dihydro-9,10-ethanoanthracene（LH4）, C10H8N2 = 4,4＇-bipyridine（bpy） and C12H10N2 = 4,4＇-bipyridinylethane（bpe）） have been obtained by mixing LH4 with corresponding bpy or bpe ligand. The two complexes have been determined by X-ray crystal structure analysis, elemental analysis and IR analysis. Compound I crystallizes in the orthorhombic Pnma with a = 9.7078（4）, b = 22.4974（10）, c = 20.6272（9） V = 4505.0（3）3, Mr = 454.51, Dc. = 1.340 g·cm^-3, μ = 0.09 mm-1, F（000） = 1920, Z = 8, R = 0.0503 and wR = 0.1360. Compound II crystallizes in monoclinic C2/c with a = 29.944（6）, b = 9.820（2）, c = 22.643（5） , V = 5048.4（18）3, Mr = 480.54, Dc. = 1.265 g cm^–3, μ = 0.084 mm^–1, F（000） = 2032, Z = 8, R = 0.0548 and wR = 0.1600. X-ray single-crystal structure analysis shows that two-dimensional（2D） layer supramolecular structures are formed through hydrogen bonds and π-π interactions in the two complexes. IR analysis also indicates that there are only associated hydroxyl groups in the two complexes.
文摘A new environmental friendly catalyst, HaSiWrMo6O40/PAn was prepared and identified by means of FT-IR, XRD and TG/DTA. The optimum conditions have been found, that was, mass ratio of m（PAn）： m（HaSiW6Mo6On.） was 1：1.25, volume of methanol was 20 mL, and the reflux reaction time was 2h. The structural identity of Keggin units was preserved after the incorporation into polyaniline matrix. H4SiW6Mo6040/PAn was used as catalyst in catalytic synthesis of acetals and ketals. Effects of n（aldehyde（ketone ））： n（glycol）, catalyst dosage and reaction time on yield were investingated. Optimal conditions were： n（aldehyde（ketone））： n（glycol）=1.0： 1.5; mass fraction of catalyst to reactants, 0.5%; reaction time, 1.0 h and cyclohexane as water-stripped reagent, 15 mL. Under these conditions, yields of actels and ketals were 31.9%-91.6%.
文摘A new method has been developed for separation and determination of zinc,copper,cobalt and nickel based on their colour chelates with 6,6″-dimethyl-4′-phenyl-2,2′:6′,2″-terpyridine（TPY） by ion pair high performance liquid chromatography in a reversed phase mode.The suitable conditions are the methanol-water（80:20,V/V） containing 10mmol/L NaH2PO4-H3PO4 buffer solution（pH=5.0） and 3.0mmol/L sodium dodecyl sulfonate as mobile phase,on a Symmetry C18 column（3.9mmID×150mm）,the flow rate of the mobile phase is 1.0mL/min.Spectrophotometric detection was made at 340nm.The detective limits are 0.05,0.10,2.00 and 0.50ng/mL respectively.The method has good selectivity and sensitivity.It has been applied to the separation and determination of zinc,copper,cobalt and nickel in human hair and tobacco and the result is satisfied.
文摘The title compound (p-methylphenylbis(4, 4-dimethyl-6-hydroxycyclohexene-1-one-2-yl)methane) has been synthesized by the reaction of 4-methylbenzaldehyde and 5, 5-dimethyl-1, 3-cyclohexanedione in N,N-dimethylformamide. Its structure was determined by single crystal X-ray diffraction. The Crystal is monoclinic, space group P21/a, a=0. 9304 (2)nm, b=1. 1754 (2)nm, c=2. 0134 (4)nm, β=102. 40(2)°, Mr= 382. 50, V=2. 1505 (7)nm3, Dc = 1. 181g/cm3, Z=4, μ(MoKα) = 0. 79cm-1, F(000) = 856.The structure was solved by direct methods, and refined by full-matris least-Squares method to a final R =0. 042 and Rw = 0. 045. The crystal structure shows that there are two conjugated enol form in the molecule.
基金Supported by the Third World Academy of Science.(TWAS Fellowship for Research and Advanced Training FR number:Grant No.3240224121the International Foundation for Science (IFS,Stockholm,Sweden) and the Organizationfor the Prohibition of Chemical Weapons(OPCW)(IFS Research Grant No F/4921-2)
文摘Objective:To isolate and characterize the cytotoxic compounds from Diospyros quercina(Baill.)G.E.Schatz&Lowry(Ebenaceae).Methods:An ethno-botanical survey was conducted in the south of Madagascar from July to August 2010.Bio-guided fractionation assay was carried out on the root bark of Diospyros quercina,using cytotoxicity bioassay on murine P388 leukemia cell lines as model.The structures of the cytotoxic compounds were elucidated by 1D and 2D NMR spectroscopy and mass spectrometry.Results:Biological experiments resulted in the isolation of three bioactive pure compounds(named TR-21,TR-22,and TR-23)which exhibited very good in vitro cytotoxic activities with the IC_(50)values of(0.017 5±0.0060)μg/mL,(0.089±0.005)μg/mL and(1.027±0.070)μg/mL respectively.Thus,they support the claims of traditional healers and suggest the possible correlation between the chemical composition of this plant and its wide use in Malagasy folk medicine to treat cancer.Conclusions:The ability of isolated compounds in this study to inhibit cell growth may represent a rational explanation for the use of Diospyros quercina root bark in treating cancer by Malagasy traditional healers.Further studies are,therefore,necessary to evaluate the in vivo antineoplastic activity of these cytotoxic compounds as effective anticancer drugs.
