Zinc chloride is an efficient and safe catalyst in the [3 ＋ 2] cycloaddition reaction of organic nitriles with sodium azide in solventless condition. The corresponding 5-substituted ^1H tetrazoles were obtained under...Zinc chloride is an efficient and safe catalyst in the [3 ＋ 2] cycloaddition reaction of organic nitriles with sodium azide in solventless condition. The corresponding 5-substituted ^1H tetrazoles were obtained under mild conditions. This method can overcome disadvantages such as： the use of toxic metals and expensive reagents, drastic reaction conditions, water sensitivity and the presence of dangerous hydrazoic acid.展开更多
Sulfonylurea herbicides have been widely used because of their low application rates, good crop sdeetivities and low mammalian toxicities. However, some sulfonylureas might persist unfavourably in the environment with...Sulfonylurea herbicides have been widely used because of their low application rates, good crop sdeetivities and low mammalian toxicities. However, some sulfonylureas might persist unfavourably in the environment with residual problems. In order to look for ecologically safer and environmentally benign sulfonylureas, and on keeping the pyrimidine ring being monosubstitated, 15 novd C5-monosubstituted benzenesulfonylurea compounds were synthesized. The structures of all the compounds synthesized were confirmed by demental analysis and ^1H NMR. Preliminary herbicidal activities of these new sulfonylurea compounds were determined by ALS screening （ in vitro） and pot bioassay experiments（ in vivo）. The herbicidal results show that some novel sulfonylureas are comparable to commercial Foramsulfuron and Monosulfuron.展开更多
Four novel 5-substituted pyridine-2(1H)-one derivatives were designed and synthesized by using addition-elimination reactions.The structures of these novelly synthesized compounds were verified by ~1H NMR,ESI-MS and s...Four novel 5-substituted pyridine-2(1H)-one derivatives were designed and synthesized by using addition-elimination reactions.The structures of these novelly synthesized compounds were verified by ~1H NMR,ESI-MS and single crystal X-ray diffraction.Furthermore,all four compounds(most notably compound 7a) were found to be highly efficient against hepatitis B virus (HBV) in cultured HepG2 2.2.15 cell,making them promising drug candidates for potential bioactive molecule against hepatitis B.展开更多
Six novel tetrazoles were designed, synthesized and characterized by NMR and elemental analysis. 2-Dehydroabietyl-5-ethylsulfanyl-1,2,3,4-tetrazole （4b）, C23H34N4S, was structurally determined by single-crystal X-ra...Six novel tetrazoles were designed, synthesized and characterized by NMR and elemental analysis. 2-Dehydroabietyl-5-ethylsulfanyl-1,2,3,4-tetrazole （4b）, C23H34N4S, was structurally determined by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group P212121, with a = 7.391（3）, b = 12.580（3）, c = 24.036（8） A^°, V= 2234.8（13） A^°^3, Z = 4, M, = 398.60, Dc = 1.185 g/cm^3, μ = 0.160 mm^-1, F（000） = 864, the final R = 0.0499 and wR = 0.0638 for 1228 observed reflections with I 〉 2σ（I）. There are four rings in the crystal structure, and C（14） adopts the R absolute configuration. In addition, disordered C（19）, C（20）, C（21）, C（22） and C（23） exist in the crystal structure.展开更多
5-Substituted hexahydro-1H-1,4-diazepine analogues were synthesized starting from N,N'-dibenzyl-1, 2-ethylenediamine and methyl 2, 4-dibromide butyrate through nucleophilic substitution, reduction, chlorination, d...5-Substituted hexahydro-1H-1,4-diazepine analogues were synthesized starting from N,N'-dibenzyl-1, 2-ethylenediamine and methyl 2, 4-dibromide butyrate through nucleophilic substitution, reduction, chlorination, debenzylation and amidation. Bioactivity tests showed that 9a had the highest agonist activity.展开更多
Additions of diethyl phosphite to α-nitroalkenes followed by the introduction of trimethylchlorosilane and an activated alkene, gave the corresponding title compounds via regioselective 1,3-dipolar cycloaddition in m...Additions of diethyl phosphite to α-nitroalkenes followed by the introduction of trimethylchlorosilane and an activated alkene, gave the corresponding title compounds via regioselective 1,3-dipolar cycloaddition in moderate yield.展开更多
An efficient and simple method for the preparation of 5-arylamino-1H-tetrazole and 1-aryl-5-amino-1H-tetrazole derivatives is reported using aluminum（Ⅲ） hydrogensulfate（Al（HSO4）3） as an effective heterogeneous ...An efficient and simple method for the preparation of 5-arylamino-1H-tetrazole and 1-aryl-5-amino-1H-tetrazole derivatives is reported using aluminum（Ⅲ） hydrogensulfate（Al（HSO4）3） as an effective heterogeneous catalyst from secondary arylcyanamides. Generally,when the substitution in arylcyanamide is strongly electron-withdrawing the position of equilibrium would shift toward the isomer of 1-aryl-5-amino-1H-tetrazole（B） and as the electron-donating of substituent increased,the position of equilibrium is shifted toward the isomer of 5-arylamino-1H-tetrazole（A）.The present methodology offers several advantages,such as excellent yields,short reaction times,easy work-up and greener conditions.展开更多
Hydrothermal reactions of 5-（tetrazol-5-yl） isophthalic acid with cadmium nitrate/praseodymium nitrate led to two complexes of [Cd3（TZI）2（H2O）（11）]n（1） and [Pr（TZI）（H2O）5]n（2）. Their structures and pro...Hydrothermal reactions of 5-（tetrazol-5-yl） isophthalic acid with cadmium nitrate/praseodymium nitrate led to two complexes of [Cd3（TZI）2（H2O）（11）]n（1） and [Pr（TZI）（H2O）5]n（2）. Their structures and properties were determined by X-ray diffraction, IR spectroscopy, fluorescence spectrum, thermal gravimetric analyses and elemental analysis. Complex 1 belongs to monoclinic system, I2/c space group, with a = 12.8688（3）, b = 18.0925（3）, c = 14.5190（3）A, β = 116.054（3）°, V =3036.92（13） A^3, Z = 4; complex 2 crystallizes in triclinic, space group P 1, with a = 7.9690（5）, b =9.7665（8）, c = 10.4353（9） A, α = 116.709（9）, β = 107.461（6）, γ = 95.671（6）°, V = 665.54（9）A^3 and Z =2. Complex 1 is a 3D planar structure. Complex 2 is a one-dimensional double chain configuration and extends into a 3D network by hydrogen bonds and π-π interactions.展开更多
A novel polymeric zinc（II） complex {[Zn2（TIA）（H2O）3]·（NO3）}n（1, H3TIA = 5-（1H-tetrazol-5-yl）isophthalic acid） has been synthesized in mixed solvents under solvothermal conditions and characterized by ...A novel polymeric zinc（II） complex {[Zn2（TIA）（H2O）3]·（NO3）}n（1, H3TIA = 5-（1H-tetrazol-5-yl）isophthalic acid） has been synthesized in mixed solvents under solvothermal conditions and characterized by elemental analysis, IR spectroscopy and X-ray single-crystal diffraction. Complex 1 crystallizes in orthorhombic, space group Cmcm with a = 10.4210（6）, b =23.3526（14）, c = 6.9214（4）A, V = 1684.37（17）A^3, Z = 4, C9H4N5O（10）Zn2, Mr = 472.91, Dc = 1.865g/cm^3, F（000） = 932, λ（MoK α） = 2.909 mm^-1, R = 0.0423 and wR = 0.1287. The complex has good thermal stability and excellent photoluminescent property.展开更多
Hydrothermal reactions of 3-cyanopyridine and Na N3 with Zn Cl_2 or Cd Cl_2·5/2H_2 O in the presence of 1,4-benzenedicarboxylic acid（H2bdc） yielded two new coordination polymers,{[Zn（3-ptz）（bdc）_（0.5）（H...Hydrothermal reactions of 3-cyanopyridine and Na N3 with Zn Cl_2 or Cd Cl_2·5/2H_2 O in the presence of 1,4-benzenedicarboxylic acid（H2bdc） yielded two new coordination polymers,{[Zn（3-ptz）（bdc）_（0.5）（H_2O）_2]n·2H_2O}_n（1） and [Cd_2（3-ptz）_2Cl_2]_n（2）,based on in situ synthesized 5-（3-pyridyl）tetrazolate（3-ptz-） organic ligand.They have been structurally characterized by elemental analysis（EA）,infrared spectroscopy（IR） and single-crystal/powder X-ray diffraction（PXRD）.In 1,two Zn（Ⅱ） ions are linked together through two μ_2-（3-ptz-） ligands to form a dimeric unit of [Zn（μ_2-3-ptz）（H_2O）_2]2^2＋,which is further connected with other equivalent units by μ_2-bdc^2-spacers,resulting in an infinite 1D polymeric chain of [Zn_2（3-ptz）_2（H_2O）_2（bdc）]_n,and then strong hydrogen bonding interactions extend these 1D chains into a 3D supramolecular structure.In 2,the Cd（Ⅱ） ions are connected through μ_4-（3-ptz-） ligands and Cl-anions,leading to infinite 2D layers of [Cd_2（3-ptz）Cl_2]_n^n＋,which are further linked by another μ_4-（3-ptz-） pillared ligand to form a 3D layered-pillared framework architecture of [Cd）2（3-ptz））2Cl）2]）n.Furthermore,thermal stability of these compounds was measured by thermogravimetric analysis（TGA） and their photoluminescent properties were also investigated in the solid state at room temperature.展开更多
We have developed simple,cost effective and environmentally benign protocol for the synthesis of 5-substituted 1H-tetrazoles via[2,3]cycloaddition reaction from organic nitriles and sodium azide in glycerol under cata...We have developed simple,cost effective and environmentally benign protocol for the synthesis of 5-substituted 1H-tetrazoles via[2,3]cycloaddition reaction from organic nitriles and sodium azide in glycerol under catalyst free condition.The corresponding 5-substituted 1H-tetrazoles were obtained with good to excellent yields（68-95%）.展开更多
基金Research Council of K.N.Toosi University of Technology for partial financial support of this work
文摘Zinc chloride is an efficient and safe catalyst in the [3 ＋ 2] cycloaddition reaction of organic nitriles with sodium azide in solventless condition. The corresponding 5-substituted ^1H tetrazoles were obtained under mild conditions. This method can overcome disadvantages such as： the use of toxic metals and expensive reagents, drastic reaction conditions, water sensitivity and the presence of dangerous hydrazoic acid.
基金Supported by the National Key Basic Research Program of China(No.2003CB114406)the National Natural Science Foundation Key Project of China(No.20432010).
文摘Sulfonylurea herbicides have been widely used because of their low application rates, good crop sdeetivities and low mammalian toxicities. However, some sulfonylureas might persist unfavourably in the environment with residual problems. In order to look for ecologically safer and environmentally benign sulfonylureas, and on keeping the pyrimidine ring being monosubstitated, 15 novd C5-monosubstituted benzenesulfonylurea compounds were synthesized. The structures of all the compounds synthesized were confirmed by demental analysis and ^1H NMR. Preliminary herbicidal activities of these new sulfonylurea compounds were determined by ALS screening （ in vitro） and pot bioassay experiments（ in vivo）. The herbicidal results show that some novel sulfonylureas are comparable to commercial Foramsulfuron and Monosulfuron.
文摘Four novel 5-substituted pyridine-2(1H)-one derivatives were designed and synthesized by using addition-elimination reactions.The structures of these novelly synthesized compounds were verified by ~1H NMR,ESI-MS and single crystal X-ray diffraction.Furthermore,all four compounds(most notably compound 7a) were found to be highly efficient against hepatitis B virus (HBV) in cultured HepG2 2.2.15 cell,making them promising drug candidates for potential bioactive molecule against hepatitis B.
基金Supported by the Foundation of 100 Young and Middle-aged Disciplinary Leaders of Guangxi Province in the 21st century (No. 2004219)the Natural Science Foundation of Guangxi Province (No. 0731054)
文摘Six novel tetrazoles were designed, synthesized and characterized by NMR and elemental analysis. 2-Dehydroabietyl-5-ethylsulfanyl-1,2,3,4-tetrazole （4b）, C23H34N4S, was structurally determined by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group P212121, with a = 7.391（3）, b = 12.580（3）, c = 24.036（8） A^°, V= 2234.8（13） A^°^3, Z = 4, M, = 398.60, Dc = 1.185 g/cm^3, μ = 0.160 mm^-1, F（000） = 864, the final R = 0.0499 and wR = 0.0638 for 1228 observed reflections with I 〉 2σ（I）. There are four rings in the crystal structure, and C（14） adopts the R absolute configuration. In addition, disordered C（19）, C（20）, C（21）, C（22） and C（23） exist in the crystal structure.
文摘5-Substituted hexahydro-1H-1,4-diazepine analogues were synthesized starting from N,N'-dibenzyl-1, 2-ethylenediamine and methyl 2, 4-dibromide butyrate through nucleophilic substitution, reduction, chlorination, debenzylation and amidation. Bioactivity tests showed that 9a had the highest agonist activity.
文摘Additions of diethyl phosphite to α-nitroalkenes followed by the introduction of trimethylchlorosilane and an activated alkene, gave the corresponding title compounds via regioselective 1,3-dipolar cycloaddition in moderate yield.
文摘An efficient and simple method for the preparation of 5-arylamino-1H-tetrazole and 1-aryl-5-amino-1H-tetrazole derivatives is reported using aluminum（Ⅲ） hydrogensulfate（Al（HSO4）3） as an effective heterogeneous catalyst from secondary arylcyanamides. Generally,when the substitution in arylcyanamide is strongly electron-withdrawing the position of equilibrium would shift toward the isomer of 1-aryl-5-amino-1H-tetrazole（B） and as the electron-donating of substituent increased,the position of equilibrium is shifted toward the isomer of 5-arylamino-1H-tetrazole（A）.The present methodology offers several advantages,such as excellent yields,short reaction times,easy work-up and greener conditions.
基金Supported by the International Science&Technology Cooperation Program of China(No.2011DFA51980)the International Scientific and Technological Cooperation Projects of Shanxi Province(No.2015081043)+1 种基金“131”Leading Talents Project in Colleges and Universities,Science and Technology Innovation Project of Shanxi Province(No.2014101002)Graduate Student Education Innovation Project of Shanxi Province(No.20141101)
文摘Hydrothermal reactions of 5-（tetrazol-5-yl） isophthalic acid with cadmium nitrate/praseodymium nitrate led to two complexes of [Cd3（TZI）2（H2O）（11）]n（1） and [Pr（TZI）（H2O）5]n（2）. Their structures and properties were determined by X-ray diffraction, IR spectroscopy, fluorescence spectrum, thermal gravimetric analyses and elemental analysis. Complex 1 belongs to monoclinic system, I2/c space group, with a = 12.8688（3）, b = 18.0925（3）, c = 14.5190（3）A, β = 116.054（3）°, V =3036.92（13） A^3, Z = 4; complex 2 crystallizes in triclinic, space group P 1, with a = 7.9690（5）, b =9.7665（8）, c = 10.4353（9） A, α = 116.709（9）, β = 107.461（6）, γ = 95.671（6）°, V = 665.54（9）A^3 and Z =2. Complex 1 is a 3D planar structure. Complex 2 is a one-dimensional double chain configuration and extends into a 3D network by hydrogen bonds and π-π interactions.
基金Supported by the National Natural Science Foundation of China(No.21576112)the Program for New Century Excellent Talents in University(NCET-10-0176)of ChinaNatural Science Foundation Project of Jilin Province(No.20130521019JH and 201215219)
文摘A novel polymeric zinc（II） complex {[Zn2（TIA）（H2O）3]·（NO3）}n（1, H3TIA = 5-（1H-tetrazol-5-yl）isophthalic acid） has been synthesized in mixed solvents under solvothermal conditions and characterized by elemental analysis, IR spectroscopy and X-ray single-crystal diffraction. Complex 1 crystallizes in orthorhombic, space group Cmcm with a = 10.4210（6）, b =23.3526（14）, c = 6.9214（4）A, V = 1684.37（17）A^3, Z = 4, C9H4N5O（10）Zn2, Mr = 472.91, Dc = 1.865g/cm^3, F（000） = 932, λ（MoK α） = 2.909 mm^-1, R = 0.0423 and wR = 0.1287. The complex has good thermal stability and excellent photoluminescent property.
基金supported by the National Natural Science Foundation of China(No.21071099)Natural Science Foundation of Guangdong Province(No.2015A030313750)Characteristic Innovation Projects Guangdong Provincial Department of Education(Natural Science Category,2014KTSCX169)
文摘Hydrothermal reactions of 3-cyanopyridine and Na N3 with Zn Cl_2 or Cd Cl_2·5/2H_2 O in the presence of 1,4-benzenedicarboxylic acid（H2bdc） yielded two new coordination polymers,{[Zn（3-ptz）（bdc）_（0.5）（H_2O）_2]n·2H_2O}_n（1） and [Cd_2（3-ptz）_2Cl_2]_n（2）,based on in situ synthesized 5-（3-pyridyl）tetrazolate（3-ptz-） organic ligand.They have been structurally characterized by elemental analysis（EA）,infrared spectroscopy（IR） and single-crystal/powder X-ray diffraction（PXRD）.In 1,two Zn（Ⅱ） ions are linked together through two μ_2-（3-ptz-） ligands to form a dimeric unit of [Zn（μ_2-3-ptz）（H_2O）_2]2^2＋,which is further connected with other equivalent units by μ_2-bdc^2-spacers,resulting in an infinite 1D polymeric chain of [Zn_2（3-ptz）_2（H_2O）_2（bdc）]_n,and then strong hydrogen bonding interactions extend these 1D chains into a 3D supramolecular structure.In 2,the Cd（Ⅱ） ions are connected through μ_4-（3-ptz-） ligands and Cl-anions,leading to infinite 2D layers of [Cd_2（3-ptz）Cl_2]_n^n＋,which are further linked by another μ_4-（3-ptz-） pillared ligand to form a 3D layered-pillared framework architecture of [Cd）2（3-ptz））2Cl）2]）n.Furthermore,thermal stability of these compounds was measured by thermogravimetric analysis（TGA） and their photoluminescent properties were also investigated in the solid state at room temperature.
基金support from Department of Atomic Energy-Board of Research in Nuclear Sciences(DAE-BRNS)(No2009/37/39/BRNS/2268)
文摘We have developed simple,cost effective and environmentally benign protocol for the synthesis of 5-substituted 1H-tetrazoles via[2,3]cycloaddition reaction from organic nitriles and sodium azide in glycerol under catalyst free condition.The corresponding 5-substituted 1H-tetrazoles were obtained with good to excellent yields（68-95%）.
