Two new coordination polymers, [Cd(N3)2(Baep)l/2]n (1) and [Cd2(N3)4(CH3OH)(Bapp)I/.2]n (2) (Baep = 1,4-bis(2-aminoethyl)piperazine, Bapp = 1,4-bis(3-aminopropyl)piperazine) were synthesized. The c...Two new coordination polymers, [Cd(N3)2(Baep)l/2]n (1) and [Cd2(N3)4(CH3OH)(Bapp)I/.2]n (2) (Baep = 1,4-bis(2-aminoethyl)piperazine, Bapp = 1,4-bis(3-aminopropyl)piperazine) were synthesized. The crystal of 1 is of monoclinic system, space group P21/c with a = 9.341(7), b = 11.677(9), c = 8.195(6) A, fl = 93.925(13), V= 891.8(11) A3, Z= 4, μ(MoKa) = 2.42 mm-1, Mr = 280.58, Dc = 2.090 g/cm3, the final R = 0.0297 and wR = 0.0720. The crystal of 2 is of triclinic system, space group PI with a = 9.121(5), b = 9.666(5), c = 10.250(6) A, a = 72.91(2), β= 77.10(2), V = 73.95(2)°, V = 820.0(8)°, Z = 2,μ(MoKa) = 2.62 mm-1, Mr= 522.10, Dc = 2.114 g/cm3, the final R = 0.0251 and wR = 0.0632. Single-crystal X-ray diffraction studies reveal that 1 is a 3D structure based on a dinuclear unit {Cd2(N3)a(Baep)}, in which the Baep ligands formed in situ display two different bridging modes. Compound 2 also has a 3D structure based on a tetranuclear cluster {Cda(N3)8(CH3OH)2(Bapp)}, in which the azido anions exhibit four different bridging modes (μ-1,1, μ-1,3, μ-l,l,1 and μ-1,1,3). The thermal stability and fluorescent property of 1 and 2 have also been investigated.展开更多
In accordance with the research specifications and guidelines in China,we developed a novel experimental method to detect new piperazine‑type drugs,such as 1‑(3‑trifluoromethylphenyl)piperazine and 1‑(3‑chlorophenyl)p...In accordance with the research specifications and guidelines in China,we developed a novel experimental method to detect new piperazine‑type drugs,such as 1‑(3‑trifluoromethylphenyl)piperazine and 1‑(3‑chlorophenyl)piperazine.In this study,a new pretreatment method and gas chromatography(GC)/nitrogen–phosphorus detector detection technique were used to characterize these two kinds of drugs in urine and blood samples.For the purpose of isolation of these trace drugs from the samples,liquid‑liquid extraction/solid‑phase extraction was modified and validated for this specific study.The pretreatment method presented in this paper has many advantages,such as high recovery rate,high extraction efficiency,high detection sensitivity,low limit of detection,and simple operation.The GC/NPD instrument is popular in most laboratories because it can meet the routine requirements of forensic science.All these aspects make this combination of sample pretreatment and GC/NPD technique the most suitable choice for drug detection in biological samples.展开更多
A series of novel furan/thiophene and piperazine-containing 1,2,4-triazole Mannich bases and bis(1,2,4-triazole) Mannich bases have been conveniently synthesized via Mannich reaction with triazole Schiff bases, vari...A series of novel furan/thiophene and piperazine-containing 1,2,4-triazole Mannich bases and bis(1,2,4-triazole) Mannich bases have been conveniently synthesized via Mannich reaction with triazole Schiff bases, various pipera- zinc derivatives, and formaldehyde as intermediates in good yields. Their structures were characterized by melting points, ~H NMR, 13C NMR, IR and elemental analysis. The preliminary bioassay showed that most compounds ex- hibited significant in vitro and in vivo fungicidal activity against several test plant fungi. Among 32 new compounds, the trifluoromethyl-containing compounds showed superior activity than the methyl-containing ones. Several com- pounds, such as FS, F9, F10, G5, HT, 118, 13 and 14, were comparable with some commercial fungicides against different fungi during the present study and could be further structurally optimized. Meanwhile, several compounds showed good herbicidal activity against Brassica campestris at 100 ~tg/mL and KARl inhibitory activity at 200 μg/mL. However, compounds exhibited poor insecticidal activity against oriental armyworm at 200 μg/mL in the preliminary studies. The research results will provide useful information for the design and discovery of new agro- chemicals with novel heterocyclic structures.展开更多
基金supported by the National Basic Research Program of China(973Program,2012CB821702)the National Natural Science Foundation of China(21173221and20903096)+1 种基金the State Key Laboratory of Structural ChemistryFujian Institute of Research onthe Structure of Matter,Chinese Academy of Sciences,Fuzhou,Fujian350002,China
文摘Two new coordination polymers, [Cd(N3)2(Baep)l/2]n (1) and [Cd2(N3)4(CH3OH)(Bapp)I/.2]n (2) (Baep = 1,4-bis(2-aminoethyl)piperazine, Bapp = 1,4-bis(3-aminopropyl)piperazine) were synthesized. The crystal of 1 is of monoclinic system, space group P21/c with a = 9.341(7), b = 11.677(9), c = 8.195(6) A, fl = 93.925(13), V= 891.8(11) A3, Z= 4, μ(MoKa) = 2.42 mm-1, Mr = 280.58, Dc = 2.090 g/cm3, the final R = 0.0297 and wR = 0.0720. The crystal of 2 is of triclinic system, space group PI with a = 9.121(5), b = 9.666(5), c = 10.250(6) A, a = 72.91(2), β= 77.10(2), V = 73.95(2)°, V = 820.0(8)°, Z = 2,μ(MoKa) = 2.62 mm-1, Mr= 522.10, Dc = 2.114 g/cm3, the final R = 0.0251 and wR = 0.0632. Single-crystal X-ray diffraction studies reveal that 1 is a 3D structure based on a dinuclear unit {Cd2(N3)a(Baep)}, in which the Baep ligands formed in situ display two different bridging modes. Compound 2 also has a 3D structure based on a tetranuclear cluster {Cda(N3)8(CH3OH)2(Bapp)}, in which the azido anions exhibit four different bridging modes (μ-1,1, μ-1,3, μ-l,l,1 and μ-1,1,3). The thermal stability and fluorescent property of 1 and 2 have also been investigated.
基金supported by Fundamental research fund of Institute of Forensic Science,Ministry of Public Security(The detection of new drugs analysis in biological samples.No.2012JB005)Academician Foundation of the Ministry of Public Security of the People’s Republic of China(No.2011-23214203,23215243,23317015)+2 种基金Beijing Municipal Education Commission University Science and Technology Park Construction Project(2011-08111603)Program for Young Innovative Research Team in China University of Political Science and Law(2014CXTD04,16CXTD05)the opening project fund of Shanghai Key Laboratory of Criminal Scene Evidence(2011-23417049).
文摘In accordance with the research specifications and guidelines in China,we developed a novel experimental method to detect new piperazine‑type drugs,such as 1‑(3‑trifluoromethylphenyl)piperazine and 1‑(3‑chlorophenyl)piperazine.In this study,a new pretreatment method and gas chromatography(GC)/nitrogen–phosphorus detector detection technique were used to characterize these two kinds of drugs in urine and blood samples.For the purpose of isolation of these trace drugs from the samples,liquid‑liquid extraction/solid‑phase extraction was modified and validated for this specific study.The pretreatment method presented in this paper has many advantages,such as high recovery rate,high extraction efficiency,high detection sensitivity,low limit of detection,and simple operation.The GC/NPD instrument is popular in most laboratories because it can meet the routine requirements of forensic science.All these aspects make this combination of sample pretreatment and GC/NPD technique the most suitable choice for drug detection in biological samples.
文摘A series of novel furan/thiophene and piperazine-containing 1,2,4-triazole Mannich bases and bis(1,2,4-triazole) Mannich bases have been conveniently synthesized via Mannich reaction with triazole Schiff bases, various pipera- zinc derivatives, and formaldehyde as intermediates in good yields. Their structures were characterized by melting points, ~H NMR, 13C NMR, IR and elemental analysis. The preliminary bioassay showed that most compounds ex- hibited significant in vitro and in vivo fungicidal activity against several test plant fungi. Among 32 new compounds, the trifluoromethyl-containing compounds showed superior activity than the methyl-containing ones. Several com- pounds, such as FS, F9, F10, G5, HT, 118, 13 and 14, were comparable with some commercial fungicides against different fungi during the present study and could be further structurally optimized. Meanwhile, several compounds showed good herbicidal activity against Brassica campestris at 100 ~tg/mL and KARl inhibitory activity at 200 μg/mL. However, compounds exhibited poor insecticidal activity against oriental armyworm at 200 μg/mL in the preliminary studies. The research results will provide useful information for the design and discovery of new agro- chemicals with novel heterocyclic structures.