The title compound2-p-methyloxyphenyl-3a-（2-phenyl-1,2,3-triazole-4-yl）-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine （C31H25N5O2S, Mr = 531.63） has been synthesized and its structure was determined b...The title compound2-p-methyloxyphenyl-3a-（2-phenyl-1,2,3-triazole-4-yl）-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine （C31H25N5O2S, Mr = 531.63） has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.888（2）, b = 15.115（3）, c = 16.702（3）A, α = 99.90（3）, β = 95.21（3）, γ = 100.41（3）°, V = 2642.1（9） nm^3, Dc = 1.336 g/cm^3, Z = 4, F（000） = 1112, μ = 0.162 mm^-1 ,λ（MoKα） = 0.071073 nm, R = 0.0357 and wR = 0.1126 for 10620 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecular backbone consists of a tricyclic system with the central seven- membered ring in a twisted boat-like conformation.展开更多
The solvothermal reaction of 3-amino-1H-1,2,4-triazole （ttr） with Zn（ClO4）2·6H2O and NaCl in a 1：1：1 molar ratio gave a new complex [Zn（ttr）Cl]n with a 3-connected （4.82） 2-D structure. The layers stack...The solvothermal reaction of 3-amino-1H-1,2,4-triazole （ttr） with Zn（ClO4）2·6H2O and NaCl in a 1：1：1 molar ratio gave a new complex [Zn（ttr）Cl]n with a 3-connected （4.82） 2-D structure. The layers stack in the -ABAB- way along the c axis with abundant hydrogen bonding interactions to form the crystal structure. The complex [Zn（ttr）Cl]n crystallizes in the orthorhombic space group Pbca with a = 9.369（1）, b = 10.049（1）, c = 11.905（1）A, V = 1120.9（3）A^3, Z = 8.00, C2N4H3ZnCl, Mr = 183.90, Dc = 2.180 g/cm^3,μ = 4.740 mm^-1, F（000） = 720, S = 1.059 and T = 293（2） K. The final R = 0.0662 and wR = 0.2457 for 956 observed reflections with Ⅰ〉 2σ（Ⅰ）, and R = 0.0689 and wR = 0.2504 for all data.展开更多
The title compound, Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-triazole-yl）-6-chloro-pyridazine） 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the tric...The title compound, Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-triazole-yl）-6-chloro-pyridazine） 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018（3）, b = 9.832（5）, c = 9.921（5）A, a = 78.270（8）, β = 74.550（8）, γ = 83.807（8）°, V = 553.1（5）A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F（000） = 281,μ（MoKα） = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ（I）. The Co（II） ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt（II） complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.展开更多
The title compound 1-（（5-（4-（4-chlorophenoxy）-2-chlorophenyl）-2,2,3-trimethyl-oxazolidin- 5-yl）methyl）-lH-1,2,4-triazole （C21H22Cl2N4O2）has been synthesized and characterized by elemental analysis, IR, 1H NM...The title compound 1-（（5-（4-（4-chlorophenoxy）-2-chlorophenyl）-2,2,3-trimethyl-oxazolidin- 5-yl）methyl）-lH-1,2,4-triazole （C21H22Cl2N4O2）has been synthesized and characterized by elemental analysis, IR, 1H NMR, MS and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.891（2）, b = 9.074（2）, c = 18.258（4）AA, α = 99.292（4）, β = 95.105（4）, γ = 108.068（3）°, C21H22Cl2N4O2, Mr = 433.33, V= 1059.3（4） Aa, Z = 2, Dc = 1.359 g/cm3, F（000） = 452,μ = 0.331 mm-1, the final R = 0.0448 and wR = 0.0994 for 3727 unique reflections. The dihedral angle between the oxazolidine ring taking an envelope conformation with a local pseudo-mirror and the triazole ring is 27.7（9）°. Weak intermolecular C-H...N hydrogen bonds and π-π interactions exist between the triazole rings of neighboring molecules, forming a three-dimensional network, which stabilizes the crystal structure. The primary biological test shows the target compound has certain fungicidal activity.展开更多
The crystal structure of the title compound 3-phenyl-6-（4-methylphenyl）-1,2,4- triazolo[4,3-b]-1,2,4-triazine （C17H13N5, Mr = 287.32） was synthesized and determined by singlecrystal X-ray diffraction. It belongs t...The crystal structure of the title compound 3-phenyl-6-（4-methylphenyl）-1,2,4- triazolo[4,3-b]-1,2,4-triazine （C17H13N5, Mr = 287.32） was synthesized and determined by singlecrystal X-ray diffraction. It belongs to monoclinic, space group P21/c, with α = 11.4038（18）, b = 11.7675（18）, c = 11.0904（18） A, β = 108.439（7）°, V = 1411.9（4） A^3, Z = 2, Dc = 1.352 g/cm^3, p = 0.085 mm^-1, F（000） = 600, R = 0.0445 and wR = 0.1041 for 2888 unique reflections with 1501 observed ones （I 〉20（I））. In the crystal structure, the triazine moiety is almost coplanar with the triazole ring, and the largest deviation for atom C（4） is -0.026 A. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.展开更多
A new 1,2,4-triazole containing cyclopropane moiety was synthesized and characterized by 1H NMR, MS and elemental analyses. The crystal structure of the title compound （C13H14FN3S, Mr= 263.33） has been determined by...A new 1,2,4-triazole containing cyclopropane moiety was synthesized and characterized by 1H NMR, MS and elemental analyses. The crystal structure of the title compound （C13H14FN3S, Mr= 263.33） has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.614（3）, b = 7.0202（14）, c = 15.556（3）A, β = 110.92（3）°, V = 1286.7（4） A3, Z = 4, F（000） = 552, D,. = 1.359 g/cm3,μ = 0.25 mm-1, the final R = 0.0336 and wR = 0.0898 for 2568 observed reflections with 1 〉 2σ（/）. A total of 10093 reflections were collected, of which 3045 were independent （Rint = 0.0268）. The herbicidal activity of the title compound was determined, and this compound displays excellent herbicidal activity against Brassica campestris.展开更多
The compound of 3,5-diazido-1,2,4-triazole was synthesized by the reaction of 2,5,2＇,5＇-tetrachloro-1,1＇-azo-1,3,4-triazole with sodium azide at 50 ℃.Its crystal structure was determined by single-crystal X-ray di...The compound of 3,5-diazido-1,2,4-triazole was synthesized by the reaction of 2,5,2＇,5＇-tetrachloro-1,1＇-azo-1,3,4-triazole with sodium azide at 50 ℃.Its crystal structure was determined by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group Cc with a=1.212 4（2） nm,b=2.342 4（5） nm,c=0.804 74（16） nm,β=125.56（3）°,V=1.859 3（6） nm3,Z=4,C2HN9,Mr=151.04,Dc=1.62 g/cm3,F（000）=912 and μ（MoKa）=0.129 mm-1,the final R=0.039 7 and wR=0.087 4.X-ray analysis indicates a stronger intermolecular hydrogen bonding,leading to the formation of a trimmer,containing a nine-membered cyclic ring with graph-set R33（9） in the compound.展开更多
The title compound, C9H9N5OS, was synthesized by the reaction of 3-（1H）-1,2,4 -triazole hydrazine with 3-methyl-2-thiophenecarboxaldehyde in ethanol. The single crystal structure has been determined by X-ray diffrac...The title compound, C9H9N5OS, was synthesized by the reaction of 3-（1H）-1,2,4 -triazole hydrazine with 3-methyl-2-thiophenecarboxaldehyde in ethanol. The single crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group P2 1/n with a = 9.5550（10）, b = 11.9847（12）, c = 10.1074（11） A,β= 112.995（2）° V= 1065.47（19） A^3, Z = 4,μ = 0.290 mm^-1, Mr= 235.27, Dc = 1.467 g/cm^3 and F（000） = 488. The structure was solved by direct methods and refined to R = 0.0449. The crystal structure involves intermolecular hydrogen bonds of N-H…O and N-H…N as well as intramolecular hydrogen bond of N-H…N. Its biological activity has also been determined showing this type of compounds has certain antibacterial activity.展开更多
Redox reaction of a mixture of CuC12·2H2O, HaPO3 and dpatrz （3,5-dipropyl- 4-amino-1,2,4-triazole） at room temperature yields one new compound, [Cu（1）（/.t2-dpatrz）aCu（1）CI2], with two independent cis- and...Redox reaction of a mixture of CuC12·2H2O, HaPO3 and dpatrz （3,5-dipropyl- 4-amino-1,2,4-triazole） at room temperature yields one new compound, [Cu（1）（/.t2-dpatrz）aCu（1）CI2], with two independent cis- and trans-propyl side chain molecules. Compound 1 crystallizes in monoclinic, space group P21/c with a = 7.474（1）, b = 17.807（1）, c = 18.851（1） A, β = 108.32（1）°, V = 2381.7（2） A3, Z = 4, C16H32CI2Cu2Ns, Mr = 534.48, Dc = 1.491 g.cm-3,μ = 2.03 mm-1, F（000） = 1104, GOOF = 1.050, the final R = 0.0445 and wR = 0.1162 for 3162 observed reflections （I 〉 2σ（I））. Compound 1 shows discrete dimeric structures （A and B） containing inversion centers and the Cu（l） ions are coordinated in triangle geometries. The isomers are connected by N-H…CI hydrogen bonds, chains with graph-set C（7） and rings R22（14） and C-H..＇Jr interactions into stair-step chains （Tapes A and B） running parallel to the [01-1] direction. The N-H…C1 hydrogen bonds result in chain and cyclic structures with graph-sets C22（17） and R34（18） linking tapes A and B to form two-dimensional networks along the [031] direction. Packing of crystal 1 is stabilized by rings R34（18） and weak C-H…C1 hydrogen bonds parallel to the [01-2] direction. Bond valence sum （BVS） and UV-Vis absorption spectra support the existence of Cu（I） ions. Compound 1 exhibits extensive green blue phosphorescence in the solid state at room temperature.展开更多
N′-（4-fluorobenzylidene）-2-（ 1H-1,2,4-triasole-1-yl） acetohydrazide was synthesized by the reaction of 4-flu- orobenzaldehyde with 2-（ 1H-1,2,4-triazole-1-yl） acetohydrazide. The structure was confirmed via ele...N′-（4-fluorobenzylidene）-2-（ 1H-1,2,4-triasole-1-yl） acetohydrazide was synthesized by the reaction of 4-flu- orobenzaldehyde with 2-（ 1H-1,2,4-triazole-1-yl） acetohydrazide. The structure was confirmed via elemental analysis, MS, ^1H NMR, IR, and X-ray diffraction. It crystallized in a monoclinic system with space group P2 （ 1 ）, α = 0.4905（1） nm, b =0. 8160（2） nm, c = 1.4105（3） nm, β =93. 33（3）°, Z=2, V=0.5636（2） nm^3, Do =1.457 Mg/m^3,μ =0. 112 mm^-1 , F（000） =256, and final R1 =0. 0685. Several intermolecular hydrogen-bond interactions existed in the crystal structure, facilitating the stabilization of the compound.展开更多
The title compound 2-(4-methylbenzoly)-3-(4-chlrolphenyl)-4-(1,2,4-triazole)-5- anilino-thiopene has been prepared and characterized by IR, EA, 1H NMR, UV, MS and X-ray analysis. It crystallizes in the triclinic syste...The title compound 2-(4-methylbenzoly)-3-(4-chlrolphenyl)-4-(1,2,4-triazole)-5- anilino-thiopene has been prepared and characterized by IR, EA, 1H NMR, UV, MS and X-ray analysis. It crystallizes in the triclinic system, space group P1 with a = 8.061(2), b = 9.981(2), c = 15.462(3) ? a = 90.96(3), b = 103.11(3), g = 106.26(3)? Mr = 470.96 (C26H19ClN4OS), V = 1158.8(4) 3, Z = 2, Dc = 1.350 g/cm3, F(000) = 488, = 0.282 mm-1, R = 0.0482 and wR = 0.1043. In the crystal lattice, there exist some intermolecular hydrogen bonds, - stacking interactions and CH贩?supramolecular interactions. In the solid state, all of the above intermolecular interactions in the title compound can stabilize the crystal structure.展开更多
A novel Schiff base was synthesized via 5-benzyl-4-amino-1,2,4-triazole-3-thione with 3-phenoxy-benzaldehyde under refluxing. The structure was characterized by elemental analysis, IR, 1H NMR, ESI-MS and single-crysta...A novel Schiff base was synthesized via 5-benzyl-4-amino-1,2,4-triazole-3-thione with 3-phenoxy-benzaldehyde under refluxing. The structure was characterized by elemental analysis, IR, 1H NMR, ESI-MS and single-crystal X-ray diffraction. This compound crystallizes in monoclinic, space group P21 /c with a = 16.0289（16）, b = 5.8022（6）, c = 20.542（2）, β = 95.667（2）o, C22 H18 N4 OS, Mr = 386.46, V = 1901.1（3）3, Z = 4, Dc = 1.347 g/cm3, F（000） = 804, μ = 0.191 mm-1, the final R = 0.0453 and wR = 0.1307 for 2456 observed reflections with I 〉 2σ（I）. The crystal packing of the compound is stabilized by classical intermolecular N–H…S hydrogen bonds. Furthermore, the biological activity to four vegetable pathogens has been tested. The title compound exhibited good fungicidal activities to Gibberlla nicotiancola.展开更多
The title compound 5-[（1H-1,2,4-triazol-1-yl）methyl]-4-（2,3-dimethoxy-benzylideneamino）- 2H-1,2,4-triazole-3（4H）-thione monohydrate 4 has been synthesized by the treatment of 4-amino-3-（ 1,2,4-triazol- 1-yl）- ...The title compound 5-[（1H-1,2,4-triazol-1-yl）methyl]-4-（2,3-dimethoxy-benzylideneamino）- 2H-1,2,4-triazole-3（4H）-thione monohydrate 4 has been synthesized by the treatment of 4-amino-3-（ 1,2,4-triazol- 1-yl）- 1 H- 1,2,4-triazole-5（4H）-thione 3 with 2,3-dimethoxybenzaldehyde. It crystallizes as a monohydrate in the triclinic system, space group P1^- with a = 8.147（2）, b = 10.820（2）, c = 10.835（2）A, α= 73.770（6）, β = 84.916（7）,γ = 70.679（6）°, C14H17N7O35, Mr = 363.41, V= 865.4（2）A^3, Z= 2, Dc = 1.395 g/cm^3, F（000） = 380, μ = 0.217 mm^-1, the final R = 0.0400 and wR = 0.0975 for 3454 unique reflections. The dihedral angles made by the thione-substituted triazole ring with the other triazole ring and benzene ring are 74.92（3） and 14.81（2）°, respectively. There are some weak hydrogen bonds and C-H..π supramolecular interactions in the lattice, forming a three-dimensional network, which stabilizes the crystal structure.展开更多
1 Introduction The Suzuki cross-coupling reaction is a powerful and versatile method for the generation of unsymmetrical biaryls from arylboronic acids and aryl halides in a single step. However, the reaction is usua...1 Introduction The Suzuki cross-coupling reaction is a powerful and versatile method for the generation of unsymmetrical biaryls from arylboronic acids and aryl halides in a single step. However, the reaction is usually performed in the presence of Pd catalyst along with phosphine ligand, which sometimes creates practical problems because organophosphines tend to be expensive, poisonous, and air sensitive. Recently, phos-phine-free ligands,展开更多
A typical nitroimine bistriazole（DNABT） was synthesized with high yield（90.4%） by nitration reaction from DABT in HNO3 and NH4NO3. Furthermore, a novel cocrystal（1） consisting of DNABT, H2O and DMSO in a 1：2：2...A typical nitroimine bistriazole（DNABT） was synthesized with high yield（90.4%） by nitration reaction from DABT in HNO3 and NH4NO3. Furthermore, a novel cocrystal（1） consisting of DNABT, H2O and DMSO in a 1：2：2 molar ratio was analysized on the crystal structure. Cocrystal 1 crystallizes in the triclinic system, space group P1 with a = 6.3124（18）, b = 8.233（2）, c = 9.775（3） A, β = 98.326（4）°, V = 481.59（74）A^3, Z = 2, Dc = 1.55 g/cm^3, F（000） = 234, μ = 0.337 mm^-1, S = 1.078, the final R = 0.0609 and w R = 0.2743. Additionally, the crystal structure is built up by four strong and seven weak hydrogen bonds. And the hydrogen bond network contributes to the stability of DNABT molecule. Typical TGA and DSC curves indicate the cocrystal 1 includes one endothermic and one exothermic decomposition processes, and the peak temperature at each process is 164.0 and 245.0 ℃. The nonisothermal decomposition kinetics analysis was performed by means of the Kissinger and Ozawa methods. The apparent activation energy（Ea） and pre-exponential factor（A） of the two decompositions are 96.0 kJ·mol^-1, 108.1 s^-1 and 215.8 kJ·mol^-1, 1018.9 s^-1, respectively.展开更多
3-Methylthio-5-hydroxy-1,2,4-triazine(1c)reacted with substituted benzenesulfonyl chloride to give 3-methylthio-5-oxy-1,2,4-triazin-6-yl pyridinium betaine(4)in anhydrous pyridine.But when NaOH/H_2O/CH_3COCH_3 or NaOH...3-Methylthio-5-hydroxy-1,2,4-triazine(1c)reacted with substituted benzenesulfonyl chloride to give 3-methylthio-5-oxy-1,2,4-triazin-6-yl pyridinium betaine(4)in anhydrous pyridine.But when NaOH/H_2O/CH_3COCH_3 or NaOH/CH_3OH were used as reactant and solvent,3-methylthio-4-substituted benzenesulfonyl-5-oxo-6-hydroxy-1,4,5,6-tetrahydro-1,2,4-triazine(6)or 1-tosyl-3-methylthio-5-oxo-6-methyloxy-1,4,5,6-tetrahydro-1,2,4-triazine(7)was obtained respectively.The above reactions show anomalous properties of nucleophilic attack on 6-carbon in 1,2,4-triazine ring.展开更多
Two aromatic multicarboxylate ligands tuned Zn(Ⅱ) coordination polymers, namely, {[Zn0.5(H2L)(tp)0.5(H2O)]H2O}n(1) and {[Zn2(HL)(btc)(H2O)]H2O}n(2)(H2L = 3-(1 Hpyrazol-4-yl)-5-(pyridin-3-yl)-1,2,4-triazole, H2tp = te...Two aromatic multicarboxylate ligands tuned Zn(Ⅱ) coordination polymers, namely, {[Zn0.5(H2L)(tp)0.5(H2O)]H2O}n(1) and {[Zn2(HL)(btc)(H2O)]H2O}n(2)(H2L = 3-(1 Hpyrazol-4-yl)-5-(pyridin-3-yl)-1,2,4-triazole, H2tp = terephthalic acid;H3 btc = 1,3,5-benzenetricarboxylic) have been synthesized. Their structures were characterized by single-crystal X-ray diffraction analysis, elemental analyses and infrared spectra. Compound 1 possesses a one-dimensional chain structure and is finally extended into a three-dimensional supramolecular architecture though hydrogen bonding interactions. Compound 2 shows a three-dimensional framework. Meanwhile, compounds 1 and 2 exhibit luminescent emission in the solid, and can be investigated as potential luminescent materials.展开更多
Covalent bioactive compounds are successfully used in clinic and attracted intense research efforts in the fundamental study as well as drug development.The advantageous effects of covalent compounds compared with non...Covalent bioactive compounds are successfully used in clinic and attracted intense research efforts in the fundamental study as well as drug development.The advantageous effects of covalent compounds compared with non-covalent ones are highly dependent on electrophilic warheads.Hence,electrophilic warheads with tunable reactivity and selectivity are highly demanded in fields of medicinal chemistry and chemical biology.Herein,we report a novel electrophilic warhead,chloromethyl group activated by thiol-substituted 1,2,4-triazole.Interestingly,a pair of regioisomers could be simultaneously occurred in the step of alkylation during the synthesis of this unique motif.This is a rare example that the alkylation could simultaneously generate these two separable regioisomers of 1,2,4-triazole at the nitrogen or sulfur atom.The covalent-working mechanism of this new warhead is confirmed by various chemoproteomics experiments including target identification and binding site mapping.Importantly,the reactivity and selectivity of this new electrophilic warhead could be efficiently tuned by virtue of stereo effect.Interestingly,one pair of regioisomers(19S and 19X)induced distinct modes of cell death.Isomer 19S could induce apoptosis of colon cancer cells while 19X could induce both apoptosis and ferroptosis.Together,this study provides pairs of novel electrophilic warheads that could be useful not only in supporting the design of covalent compounds for drug discovery but also in providing chemical probes for the fundamental biological study.展开更多
The title compound 4-（5-（（2,4-dichlorobenzyl）thio）-4-phenyl-4H-1,2,4-triazol-3- yl）pyridine （C20HI4CI2N4S） was synthesized, and its structure was confirmed by 1H NMR, MS, elemental analyses and X-ray diffracti...The title compound 4-（5-（（2,4-dichlorobenzyl）thio）-4-phenyl-4H-1,2,4-triazol-3- yl）pyridine （C20HI4CI2N4S） was synthesized, and its structure was confirmed by 1H NMR, MS, elemental analyses and X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 14.885（5）, b = 8.597（2）, c = 16.144（5）A,β= 114.505（4）°, V= 1879.8（10） A3, Z= 8 and R = 0.0320 for 3108 observed reflections with I 〉 2σ（I）. The preliminary biological test shows that the title compound has activities against Stemphylium lyeopersici （Enjoji） Yamamoto, Fusarium oxysporum, sp. cueumebrium, and Botrytis cinerea with inhibitory to be 53.57%, 66.67% and 24.44%, respectively.展开更多
基金This work was supported by the National Natural Science Foundation of China (No. 29702007 and 20162004)
文摘The title compound2-p-methyloxyphenyl-3a-（2-phenyl-1,2,3-triazole-4-yl）-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine （C31H25N5O2S, Mr = 531.63） has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.888（2）, b = 15.115（3）, c = 16.702（3）A, α = 99.90（3）, β = 95.21（3）, γ = 100.41（3）°, V = 2642.1（9） nm^3, Dc = 1.336 g/cm^3, Z = 4, F（000） = 1112, μ = 0.162 mm^-1 ,λ（MoKα） = 0.071073 nm, R = 0.0357 and wR = 0.1126 for 10620 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecular backbone consists of a tricyclic system with the central seven- membered ring in a twisted boat-like conformation.
基金The project was supported by the NNSFC (20571075, 20521101)the NSF for Distinguished Young Scientists of China (20425104) the NSF of Fujian Province (A0420002)
文摘The solvothermal reaction of 3-amino-1H-1,2,4-triazole （ttr） with Zn（ClO4）2·6H2O and NaCl in a 1：1：1 molar ratio gave a new complex [Zn（ttr）Cl]n with a 3-connected （4.82） 2-D structure. The layers stack in the -ABAB- way along the c axis with abundant hydrogen bonding interactions to form the crystal structure. The complex [Zn（ttr）Cl]n crystallizes in the orthorhombic space group Pbca with a = 9.369（1）, b = 10.049（1）, c = 11.905（1）A, V = 1120.9（3）A^3, Z = 8.00, C2N4H3ZnCl, Mr = 183.90, Dc = 2.180 g/cm^3,μ = 4.740 mm^-1, F（000） = 720, S = 1.059 and T = 293（2） K. The final R = 0.0662 and wR = 0.2457 for 956 observed reflections with Ⅰ〉 2σ（Ⅰ）, and R = 0.0689 and wR = 0.2504 for all data.
文摘The title compound, Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-triazole-yl）-6-chloro-pyridazine） 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018（3）, b = 9.832（5）, c = 9.921（5）A, a = 78.270（8）, β = 74.550（8）, γ = 83.807（8）°, V = 553.1（5）A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F（000） = 281,μ（MoKα） = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ（I）. The Co（II） ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt（II） complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.
文摘The title compound 1-（（5-（4-（4-chlorophenoxy）-2-chlorophenyl）-2,2,3-trimethyl-oxazolidin- 5-yl）methyl）-lH-1,2,4-triazole （C21H22Cl2N4O2）has been synthesized and characterized by elemental analysis, IR, 1H NMR, MS and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.891（2）, b = 9.074（2）, c = 18.258（4）AA, α = 99.292（4）, β = 95.105（4）, γ = 108.068（3）°, C21H22Cl2N4O2, Mr = 433.33, V= 1059.3（4） Aa, Z = 2, Dc = 1.359 g/cm3, F（000） = 452,μ = 0.331 mm-1, the final R = 0.0448 and wR = 0.0994 for 3727 unique reflections. The dihedral angle between the oxazolidine ring taking an envelope conformation with a local pseudo-mirror and the triazole ring is 27.7（9）°. Weak intermolecular C-H...N hydrogen bonds and π-π interactions exist between the triazole rings of neighboring molecules, forming a three-dimensional network, which stabilizes the crystal structure. The primary biological test shows the target compound has certain fungicidal activity.
基金The project was supported by the NNSFC (20572057) and NSF of Shandong Province (Y2006B011)
文摘The crystal structure of the title compound 3-phenyl-6-（4-methylphenyl）-1,2,4- triazolo[4,3-b]-1,2,4-triazine （C17H13N5, Mr = 287.32） was synthesized and determined by singlecrystal X-ray diffraction. It belongs to monoclinic, space group P21/c, with α = 11.4038（18）, b = 11.7675（18）, c = 11.0904（18） A, β = 108.439（7）°, V = 1411.9（4） A^3, Z = 2, Dc = 1.352 g/cm^3, p = 0.085 mm^-1, F（000） = 600, R = 0.0445 and wR = 0.1041 for 2888 unique reflections with 1501 observed ones （I 〉20（I））. In the crystal structure, the triazine moiety is almost coplanar with the triazole ring, and the largest deviation for atom C（4） is -0.026 A. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.
基金Supported by the National Natural Science Foundation of China(No.21002090)the Key Innovation Team of Science and Technology in Zhejiang Province(2010R50018-06)the National Key Technologies R&D Program(2011BAE06B03-01)
文摘A new 1,2,4-triazole containing cyclopropane moiety was synthesized and characterized by 1H NMR, MS and elemental analyses. The crystal structure of the title compound （C13H14FN3S, Mr= 263.33） has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.614（3）, b = 7.0202（14）, c = 15.556（3）A, β = 110.92（3）°, V = 1286.7（4） A3, Z = 4, F（000） = 552, D,. = 1.359 g/cm3,μ = 0.25 mm-1, the final R = 0.0336 and wR = 0.0898 for 2568 observed reflections with 1 〉 2σ（/）. A total of 10093 reflections were collected, of which 3045 were independent （Rint = 0.0268）. The herbicidal activity of the title compound was determined, and this compound displays excellent herbicidal activity against Brassica campestris.
基金Supported by the Program for New Century Excellent Talentsin University (NCET-09-0046)
文摘The compound of 3,5-diazido-1,2,4-triazole was synthesized by the reaction of 2,5,2＇,5＇-tetrachloro-1,1＇-azo-1,3,4-triazole with sodium azide at 50 ℃.Its crystal structure was determined by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group Cc with a=1.212 4（2） nm,b=2.342 4（5） nm,c=0.804 74（16） nm,β=125.56（3）°,V=1.859 3（6） nm3,Z=4,C2HN9,Mr=151.04,Dc=1.62 g/cm3,F（000）=912 and μ（MoKa）=0.129 mm-1,the final R=0.039 7 and wR=0.087 4.X-ray analysis indicates a stronger intermolecular hydrogen bonding,leading to the formation of a trimmer,containing a nine-membered cyclic ring with graph-set R33（9） in the compound.
基金This work was supported by the Natural Science Foundation of Zhejiang Province (No. M203115) and Scientific Research Fund of Zhejiang Provincial Education Department(NO.20050057)
文摘The title compound, C9H9N5OS, was synthesized by the reaction of 3-（1H）-1,2,4 -triazole hydrazine with 3-methyl-2-thiophenecarboxaldehyde in ethanol. The single crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group P2 1/n with a = 9.5550（10）, b = 11.9847（12）, c = 10.1074（11） A,β= 112.995（2）° V= 1065.47（19） A^3, Z = 4,μ = 0.290 mm^-1, Mr= 235.27, Dc = 1.467 g/cm^3 and F（000） = 488. The structure was solved by direct methods and refined to R = 0.0449. The crystal structure involves intermolecular hydrogen bonds of N-H…O and N-H…N as well as intramolecular hydrogen bond of N-H…N. Its biological activity has also been determined showing this type of compounds has certain antibacterial activity.
基金Supported by the National Natural Science Foundation of China(Nos.21171109&21271121)SRFDP(Nos.20111401110002&20121401110005)Shanxi Scholarship Council of China(2012-004&2013-026)
文摘Redox reaction of a mixture of CuC12·2H2O, HaPO3 and dpatrz （3,5-dipropyl- 4-amino-1,2,4-triazole） at room temperature yields one new compound, [Cu（1）（/.t2-dpatrz）aCu（1）CI2], with two independent cis- and trans-propyl side chain molecules. Compound 1 crystallizes in monoclinic, space group P21/c with a = 7.474（1）, b = 17.807（1）, c = 18.851（1） A, β = 108.32（1）°, V = 2381.7（2） A3, Z = 4, C16H32CI2Cu2Ns, Mr = 534.48, Dc = 1.491 g.cm-3,μ = 2.03 mm-1, F（000） = 1104, GOOF = 1.050, the final R = 0.0445 and wR = 0.1162 for 3162 observed reflections （I 〉 2σ（I））. Compound 1 shows discrete dimeric structures （A and B） containing inversion centers and the Cu（l） ions are coordinated in triangle geometries. The isomers are connected by N-H…CI hydrogen bonds, chains with graph-set C（7） and rings R22（14） and C-H..＇Jr interactions into stair-step chains （Tapes A and B） running parallel to the [01-1] direction. The N-H…C1 hydrogen bonds result in chain and cyclic structures with graph-sets C22（17） and R34（18） linking tapes A and B to form two-dimensional networks along the [031] direction. Packing of crystal 1 is stabilized by rings R34（18） and weak C-H…C1 hydrogen bonds parallel to the [01-2] direction. Bond valence sum （BVS） and UV-Vis absorption spectra support the existence of Cu（I） ions. Compound 1 exhibits extensive green blue phosphorescence in the solid state at room temperature.
文摘N′-（4-fluorobenzylidene）-2-（ 1H-1,2,4-triasole-1-yl） acetohydrazide was synthesized by the reaction of 4-flu- orobenzaldehyde with 2-（ 1H-1,2,4-triazole-1-yl） acetohydrazide. The structure was confirmed via elemental analysis, MS, ^1H NMR, IR, and X-ray diffraction. It crystallized in a monoclinic system with space group P2 （ 1 ）, α = 0.4905（1） nm, b =0. 8160（2） nm, c = 1.4105（3） nm, β =93. 33（3）°, Z=2, V=0.5636（2） nm^3, Do =1.457 Mg/m^3,μ =0. 112 mm^-1 , F（000） =256, and final R1 =0. 0685. Several intermolecular hydrogen-bond interactions existed in the crystal structure, facilitating the stabilization of the compound.
基金This work was supported by the Natural Science Foundation of Shandong Province (No. Y2002B06)
文摘The title compound 2-(4-methylbenzoly)-3-(4-chlrolphenyl)-4-(1,2,4-triazole)-5- anilino-thiopene has been prepared and characterized by IR, EA, 1H NMR, UV, MS and X-ray analysis. It crystallizes in the triclinic system, space group P1 with a = 8.061(2), b = 9.981(2), c = 15.462(3) ? a = 90.96(3), b = 103.11(3), g = 106.26(3)? Mr = 470.96 (C26H19ClN4OS), V = 1158.8(4) 3, Z = 2, Dc = 1.350 g/cm3, F(000) = 488, = 0.282 mm-1, R = 0.0482 and wR = 0.1043. In the crystal lattice, there exist some intermolecular hydrogen bonds, - stacking interactions and CH贩?supramolecular interactions. In the solid state, all of the above intermolecular interactions in the title compound can stabilize the crystal structure.
基金supported by the National Natural Science Foundation of China(No.21073141)the Shaanxi Provincial Education Department Foundation(No.2013JK0666)
文摘A novel Schiff base was synthesized via 5-benzyl-4-amino-1,2,4-triazole-3-thione with 3-phenoxy-benzaldehyde under refluxing. The structure was characterized by elemental analysis, IR, 1H NMR, ESI-MS and single-crystal X-ray diffraction. This compound crystallizes in monoclinic, space group P21 /c with a = 16.0289（16）, b = 5.8022（6）, c = 20.542（2）, β = 95.667（2）o, C22 H18 N4 OS, Mr = 386.46, V = 1901.1（3）3, Z = 4, Dc = 1.347 g/cm3, F（000） = 804, μ = 0.191 mm-1, the final R = 0.0453 and wR = 0.1307 for 2456 observed reflections with I 〉 2σ（I）. The crystal packing of the compound is stabilized by classical intermolecular N–H…S hydrogen bonds. Furthermore, the biological activity to four vegetable pathogens has been tested. The title compound exhibited good fungicidal activities to Gibberlla nicotiancola.
文摘The title compound 5-[（1H-1,2,4-triazol-1-yl）methyl]-4-（2,3-dimethoxy-benzylideneamino）- 2H-1,2,4-triazole-3（4H）-thione monohydrate 4 has been synthesized by the treatment of 4-amino-3-（ 1,2,4-triazol- 1-yl）- 1 H- 1,2,4-triazole-5（4H）-thione 3 with 2,3-dimethoxybenzaldehyde. It crystallizes as a monohydrate in the triclinic system, space group P1^- with a = 8.147（2）, b = 10.820（2）, c = 10.835（2）A, α= 73.770（6）, β = 84.916（7）,γ = 70.679（6）°, C14H17N7O35, Mr = 363.41, V= 865.4（2）A^3, Z= 2, Dc = 1.395 g/cm^3, F（000） = 380, μ = 0.217 mm^-1, the final R = 0.0400 and wR = 0.0975 for 3454 unique reflections. The dihedral angles made by the thione-substituted triazole ring with the other triazole ring and benzene ring are 74.92（3） and 14.81（2）°, respectively. There are some weak hydrogen bonds and C-H..π supramolecular interactions in the lattice, forming a three-dimensional network, which stabilizes the crystal structure.
基金Supported by the Zhejiang Province Natural Science Foundation,China(No.Y407240)
文摘1 Introduction The Suzuki cross-coupling reaction is a powerful and versatile method for the generation of unsymmetrical biaryls from arylboronic acids and aryl halides in a single step. However, the reaction is usually performed in the presence of Pd catalyst along with phosphine ligand, which sometimes creates practical problems because organophosphines tend to be expensive, poisonous, and air sensitive. Recently, phos-phine-free ligands,
文摘A typical nitroimine bistriazole（DNABT） was synthesized with high yield（90.4%） by nitration reaction from DABT in HNO3 and NH4NO3. Furthermore, a novel cocrystal（1） consisting of DNABT, H2O and DMSO in a 1：2：2 molar ratio was analysized on the crystal structure. Cocrystal 1 crystallizes in the triclinic system, space group P1 with a = 6.3124（18）, b = 8.233（2）, c = 9.775（3） A, β = 98.326（4）°, V = 481.59（74）A^3, Z = 2, Dc = 1.55 g/cm^3, F（000） = 234, μ = 0.337 mm^-1, S = 1.078, the final R = 0.0609 and w R = 0.2743. Additionally, the crystal structure is built up by four strong and seven weak hydrogen bonds. And the hydrogen bond network contributes to the stability of DNABT molecule. Typical TGA and DSC curves indicate the cocrystal 1 includes one endothermic and one exothermic decomposition processes, and the peak temperature at each process is 164.0 and 245.0 ℃. The nonisothermal decomposition kinetics analysis was performed by means of the Kissinger and Ozawa methods. The apparent activation energy（Ea） and pre-exponential factor（A） of the two decompositions are 96.0 kJ·mol^-1, 108.1 s^-1 and 215.8 kJ·mol^-1, 1018.9 s^-1, respectively.
基金Director of the project supported by National Natural Science foundation of China.
文摘3-Methylthio-5-hydroxy-1,2,4-triazine(1c)reacted with substituted benzenesulfonyl chloride to give 3-methylthio-5-oxy-1,2,4-triazin-6-yl pyridinium betaine(4)in anhydrous pyridine.But when NaOH/H_2O/CH_3COCH_3 or NaOH/CH_3OH were used as reactant and solvent,3-methylthio-4-substituted benzenesulfonyl-5-oxo-6-hydroxy-1,4,5,6-tetrahydro-1,2,4-triazine(6)or 1-tosyl-3-methylthio-5-oxo-6-methyloxy-1,4,5,6-tetrahydro-1,2,4-triazine(7)was obtained respectively.The above reactions show anomalous properties of nucleophilic attack on 6-carbon in 1,2,4-triazine ring.
基金financially supported by the National Natural Science Foundation of China(21571093)
文摘Two aromatic multicarboxylate ligands tuned Zn(Ⅱ) coordination polymers, namely, {[Zn0.5(H2L)(tp)0.5(H2O)]H2O}n(1) and {[Zn2(HL)(btc)(H2O)]H2O}n(2)(H2L = 3-(1 Hpyrazol-4-yl)-5-(pyridin-3-yl)-1,2,4-triazole, H2tp = terephthalic acid;H3 btc = 1,3,5-benzenetricarboxylic) have been synthesized. Their structures were characterized by single-crystal X-ray diffraction analysis, elemental analyses and infrared spectra. Compound 1 possesses a one-dimensional chain structure and is finally extended into a three-dimensional supramolecular architecture though hydrogen bonding interactions. Compound 2 shows a three-dimensional framework. Meanwhile, compounds 1 and 2 exhibit luminescent emission in the solid, and can be investigated as potential luminescent materials.
基金The National Natural Science Foundation of China(No.22177136)CAMS Innovation Fund for Medical Sciences(CIFMS,Nos.CIFMS-2021-I2M-1-007,2022-I2M-2-002)。
文摘Covalent bioactive compounds are successfully used in clinic and attracted intense research efforts in the fundamental study as well as drug development.The advantageous effects of covalent compounds compared with non-covalent ones are highly dependent on electrophilic warheads.Hence,electrophilic warheads with tunable reactivity and selectivity are highly demanded in fields of medicinal chemistry and chemical biology.Herein,we report a novel electrophilic warhead,chloromethyl group activated by thiol-substituted 1,2,4-triazole.Interestingly,a pair of regioisomers could be simultaneously occurred in the step of alkylation during the synthesis of this unique motif.This is a rare example that the alkylation could simultaneously generate these two separable regioisomers of 1,2,4-triazole at the nitrogen or sulfur atom.The covalent-working mechanism of this new warhead is confirmed by various chemoproteomics experiments including target identification and binding site mapping.Importantly,the reactivity and selectivity of this new electrophilic warhead could be efficiently tuned by virtue of stereo effect.Interestingly,one pair of regioisomers(19S and 19X)induced distinct modes of cell death.Isomer 19S could induce apoptosis of colon cancer cells while 19X could induce both apoptosis and ferroptosis.Together,this study provides pairs of novel electrophilic warheads that could be useful not only in supporting the design of covalent compounds for drug discovery but also in providing chemical probes for the fundamental biological study.
基金supported by National Natural Science Foundation of China(No.21002090)the Key Innovation Team of Science and Technology in Zhejiang Province(2010R50018-06)the National Key Technologies R&D Program(2011BAE06B03-01)
文摘The title compound 4-（5-（（2,4-dichlorobenzyl）thio）-4-phenyl-4H-1,2,4-triazol-3- yl）pyridine （C20HI4CI2N4S） was synthesized, and its structure was confirmed by 1H NMR, MS, elemental analyses and X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 14.885（5）, b = 8.597（2）, c = 16.144（5）A,β= 114.505（4）°, V= 1879.8（10） A3, Z= 8 and R = 0.0320 for 3108 observed reflections with I 〉 2σ（I）. The preliminary biological test shows that the title compound has activities against Stemphylium lyeopersici （Enjoji） Yamamoto, Fusarium oxysporum, sp. cueumebrium, and Botrytis cinerea with inhibitory to be 53.57%, 66.67% and 24.44%, respectively.
