2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl ...2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl chloride catalysts the reaction is limited to give only 1,8-dioxo-octahydroxanthenes 3a-k in very good yields.展开更多
The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determin...The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.展开更多
Solvothermal reactions of 3,5-dimethyl-2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl) pyridine (L), 1,4-benzendicarboxylic acid (H2bdc), and transitional metal cations of M11 (M = Mn, Co, Cd) in the presence of oxa...Solvothermal reactions of 3,5-dimethyl-2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl) pyridine (L), 1,4-benzendicarboxylic acid (H2bdc), and transitional metal cations of M11 (M = Mn, Co, Cd) in the presence of oxalic acid (H2ox) afford three novel supramolecular polymers (CPs), namely, {[M2(ox)(L)2][bdc][M2(Hox)2(OH)(H2O)4]·3H2O}n (M = Mn for 1, Co for 2, Cd for 3). Single-crystal X-ray diffraction analysis reveals that complexes 1-3 are isostructural and the 3D supramolecular structure was connected through non-covalent interactions. With the help of H2ox, the L ligands cheated with center atoms forming a butterfly [M2(ox)(L)2]2+ building block. The bdc2- ligand linked with the unprecedented [M2(Hox)2(OH)2(H2O)4] units through strong O-H...O hydrogen bonds forming a zigzag chain, which are further connected through π-π interactions between L and bdc2- ligands to form a 3D supramolecular structure. Moreover, elemental analyses, IR, thermogravimetric, PXRD and luminescence have been investigated.展开更多
The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its...The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6)A, α = 112.566(1), β = 92.324(2), γ = 102.91(1)°, V= 1315.65(10) A^3, Z = 2, Dc = 1.344 g/cm^3,μ(MoKa) = 0.282 mm^-1, λ = 0.71073 A, F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C( 12)-H(12)…O(1) and C(28)-H(28)...O(1)# 1 hydrogen bonds were observed in the title compound.展开更多
The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkali...The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkaline hydrolysis and nitrosation reactions. The yield of DMNNDO was increased from 37% to 45%. The structure of DMNNDO was characterized by IR,^1H NMR,^13 C NMR,and elemental analysis. Also the thermal decomposition of DMNNDO was studied by using DSC and TG-DTG to find that there are primarily two exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists as a dimeric form due to the presence of nitroso group. The crystal belongs to monoclinic system,space group C2/c with a = 14.515(3),b = 9.955(2),c = 11.897(2) °,β = 98.500(3)°,V = 1.6998(2) nm^3,Z = 8,D_c = 1.486 g×cm^-3,μ = 0.128 mm^-1,F(000) = 800,S = 1.055,R = 0.0358 and wR = 0.0917. In particular,DMNNDO could be easily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl_3 was revealed by means of NMR monitoring.展开更多
Dimethyl-1-(1, 2, 4-triazol) -2- butanone was treated with aqueous formaldehyde to give an additional product, and subsequent elimination by acetic anhydride yielded 4, 4-dimethyl-2-(1, 2, 4-triazol)-1-penten-3-one. ...Dimethyl-1-(1, 2, 4-triazol) -2- butanone was treated with aqueous formaldehyde to give an additional product, and subsequent elimination by acetic anhydride yielded 4, 4-dimethyl-2-(1, 2, 4-triazol)-1-penten-3-one. Further addition with substituted amines provided a series of (1, 2, 4-triazol)-4, 4-dimethyl-3-pentanone, which were then reduced by KBH4 to obtain a series of (1, 2, 4-triazol)-4, 4-dimethyl-3-pentanol. Their structures were confirmed by 1HNMR and elemental analysis. The results of bioassay showed that the title products possess good fungicidal activities.展开更多
Three new crystalline compounds 1-3 were successfully obtained by the reactions of 3,3'-dimethoxy-6,6'-dimethyl-2,2'-bipyridine ligand(dmbp) with the corresponding Cu(Ⅰ) salts.Crystal data for 1:orthorhombic ...Three new crystalline compounds 1-3 were successfully obtained by the reactions of 3,3'-dimethoxy-6,6'-dimethyl-2,2'-bipyridine ligand(dmbp) with the corresponding Cu(Ⅰ) salts.Crystal data for 1:orthorhombic Pbca,a = 18.5858(12),b = 8.1821(5),c = 20.6066(13) ,V = 3133.7(3) 3,Z = 8,Dc = 1.843 g/cm3,F(000) = 1696,μ = 3.366 mm-1,the final R = 0.0223 and wR = 0.0542.Crystal data for 2:Orthorhombic Pbca,a = 18.7883(16),b = 8.3249(7),c = 19.0294(17) ,V = 2976.4(4) 3,Z = 8,Dc = 1.731 g/cm3,F(000) = 1552,μ = 4.154 mm-1,the final R = 0.0279 and wR = 0.0680.Crystal data for 3:monoclinic P21/c,a = 13.812(10),b = 9.910(7),c = 23.444(17) ,β = 104.3350(10)°,V = 3090(4) 3,Z = 4,Dc = 1.476 g/cm3,F(000) = 1408,μ = 1.588 mm-1,the final R = 0.0479 and wR = 0.1081.The results of X-ray crystallographic analysis revealed that C14H16ICuN2O2(1) and C14H16BrCuN2O2(2) are isostructural compounds with the dimers connected by C-H···halogen hydrogen bonds to generate a three-dimensional(3D) supramolecular network in 1 and a two-dimensional(2D) sheet structure in 2,respectively,while the mononuclear complex C28H32Cl2Cu2N4O4(3) is ionic.In 3,the [Cu(dmbp)2]+ cations and [ClCuCl]-anions are connected by C-H···Cl hydrogen bonds to form a one-dimensional(1D) chain along the a axis.Therefore,in the three complexes,the C-H···halogen hydrogen bonds dominate their crystal structures.Additionally,The UV luminescent properties of complexes 1-3 were investigated.展开更多
Started from 5-hydroxy-2-pentanone, (R)(E)-3,7-dimethyl-2-octene-1,8-dioic acid, callosobruchusic acid, was synthesized via five steps with D-(-)-camphor sultam as the chiral auxiliary. It was of good optical purity a...Started from 5-hydroxy-2-pentanone, (R)(E)-3,7-dimethyl-2-octene-1,8-dioic acid, callosobruchusic acid, was synthesized via five steps with D-(-)-camphor sultam as the chiral auxiliary. It was of good optical purity and yield.展开更多
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
The title compound, (E)-1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)- 3-(2-methoxyphenyl)-2-(1H-1,2,4-triazol-1-yl)propenol (3a), was synthesized by the Aldol con- densation reaction of 1-(7-methox...The title compound, (E)-1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)- 3-(2-methoxyphenyl)-2-(1H-1,2,4-triazol-1-yl)propenol (3a), was synthesized by the Aldol con- densation reaction of 1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)-2-(1,2,4-triazol- 1-yl)ethanone with 2-methoxybenzaldehyde and then reduced with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction: monoclinic system, space group P21 with a = 6.2002(3), b = 12.8452(7), c = 13.2257(7) ?, Z = 2, V = 1031.23(9) ?3, Mr = 407.46, Dc = 1.312 Mg/m3, S = 1.054, μ = 0.091 mm-1, F(000) = 432, the final R = 0.0353 and wR = 0.0769 for 3161 observed reflections (I 〉 2σ(I)). X-ray analysis displays that the title compound adopts an E configuration for the C(7)=C(8) double bond and S configuration for the chirality center with the specific rotation of –63.75°. Furthermore, the stability of the crystal was maintained through the intermolecular hydrogen bond O(1)–H???N(3). The antitumor assay exhibits that the title compound 3a (E configuration) has a good antitumor activity against the Hela cell line with the IC50 value of 36.9 μM, which is better than that of 3b (Z configuration).展开更多
The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect...The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150(3), b = 9.906(3), c = 13.624(4) A, β = 106.360(4)°, V= 1443.9(7) ,A^3, Z = 4, Dc = 1.294 g/cm^3, F(000) = 592,μ(MoKa) = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O(2)-C(10) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0026 A) with the dihedral angle between them of 6.3°.展开更多
Novel polycarbonates from 5-allyloxy-1, 3-dioxan-2-one (ATMC) with 5, 5-dimethyl- 1, 3-dioxan-2-one (DTC) were successfully synthesized for the first time using immobilized porcine pancreas lipase (IPPL) as cata...Novel polycarbonates from 5-allyloxy-1, 3-dioxan-2-one (ATMC) with 5, 5-dimethyl- 1, 3-dioxan-2-one (DTC) were successfully synthesized for the first time using immobilized porcine pancreas lipase (IPPL) as catalyst. The resulting copolymers were characterized by IR, ^1H NMR, ^13C NMR and GPC. The molecular weight (Mn) of the copolymer with molar feed ratio of 10:90 (ATMC:DTC) was 9300 and the polydispersity was 1.31, while the Mn increased to 14300 and polydispersity of 1.25 with the feed ratio of 50:50. Moreover, the composition of the copolymers agreed well with the monomer feed.展开更多
从草苁蓉75%乙醇提取物中分离得到了2个单萜苷类化合物,结合其理化性质,并通过1DNMR(1 H NMR,13 C NMR)及1 H-1 H COSY、HSQC、HMBC、NOESY等多种波谱学方法进行结构鉴定,鉴定2个化合物分别为β-D-glucopyranose 1-(3,7-dimethyl-2-tran...从草苁蓉75%乙醇提取物中分离得到了2个单萜苷类化合物,结合其理化性质,并通过1DNMR(1 H NMR,13 C NMR)及1 H-1 H COSY、HSQC、HMBC、NOESY等多种波谱学方法进行结构鉴定,鉴定2个化合物分别为β-D-glucopyranose 1-(3,7-dimethyl-2-trans-6-octa-dienoate)(化合物1)和6,7-dihydrofoliamenthoic acid diglucoside(化合物2),其中化合物1为新化合物,化合物2为第1次从列当科植物中获得.展开更多
In this study,the performance of 3,5-dimethyl-2,4-dichlorophenol(DCMX) degradation by a screened strain was investigated.18 S r DNA and the neighbor-joining method were used for identification of the isolated strain...In this study,the performance of 3,5-dimethyl-2,4-dichlorophenol(DCMX) degradation by a screened strain was investigated.18 S r DNA and the neighbor-joining method were used for identification of the isolated strain.The results of phylogenetic analysis and scanning electron micrographs showed that the most probable identity of the screened strain should be Penicillium sp.Growth characteristics of Penicillium sp.and degradation processes of DCMX were examined.Fourier transform infrared spectroscopy of the inoculated DCMX solution was recorded,which supported the capacity of DCMX degradation by the screened Penicillium sp.Under different salinity conditions,the highest growth rate and removal efficiency for DCMX were obtained at p H 6.0.The removal efficiency decreased from 100%to 66% when the DCMX concentration increased from 5 to 60 mg/L,respectively.Using a Box–Behnken design,the maximum DCMX removal efficiency was determined to be 98.4%.With acclimation to salinity,higher removal efficiency could be achieved.The results demonstrate that the screened Penicillium sp.has the capability for degradation of DCMX.展开更多
A combination of HBr and trans-3,5-dihydroperoxy-3,5-dimethyl-1,2-dioxolane as anew and powerful oxidant was found effective for facile brotnination of different aromatic compounds at room temperature in water as a gr...A combination of HBr and trans-3,5-dihydroperoxy-3,5-dimethyl-1,2-dioxolane as anew and powerful oxidant was found effective for facile brotnination of different aromatic compounds at room temperature in water as a green solvent.Mild reaction conditions,high selectivity and yield,high reaction rate and non-toxicity are some of the major advantages of this synthetic protocol.展开更多
Compact and high reliable blue coherent light sources are required for the optical data storage of high density, color image processing and optical measurements.One of the possible approaches is the direct frequency d...Compact and high reliable blue coherent light sources are required for the optical data storage of high density, color image processing and optical measurements.One of the possible approaches is the direct frequency doubling of the near infrared semiconductor laser by optical waveguide techniques. So a material applied to the second harmonic generation (SHG) must not only have high molecular hyperpolarizability (β) but also have complete transparency at both the展开更多
Two novel constituents were isolated from the roots of Chinese medicinal herbs, Salvia miltiorrhiza. Their structures were determined by spectroscopic technique. The compounds were named 13,14-dihydroxy-15-methyl-benz...Two novel constituents were isolated from the roots of Chinese medicinal herbs, Salvia miltiorrhiza. Their structures were determined by spectroscopic technique. The compounds were named 13,14-dihydroxy-15-methyl-benzo[2,3-a]-7,7-dimethyl-12-oxa-tricyclo[4,4,21.4,0]dodecane(1) and 16-methyl-tropono[2,3-c]-7,7-dimethyl-12-oxa-tricyclo[4,4,21.4,0]dodecane(2).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
Objective: To isolate bioactive compounds from the endophytic fungus Fusarium sporotrichioides isolated from Rauwolfia yunnanensis, and investigate their pharmacological activities.Methods: The chemical constituents w...Objective: To isolate bioactive compounds from the endophytic fungus Fusarium sporotrichioides isolated from Rauwolfia yunnanensis, and investigate their pharmacological activities.Methods: The chemical constituents were isolated and purified by combining with ODS column chromatography, silica gel column chromatography and by performing semipreparative HPLC. Their structures were established on the basis of 1D NMR(1H-NMR and13C-NMR) and 2D NMR(1H–1H COSY,HSQC, HMBC and NOESY), as well as HRESIMS and comparison with literature data. In addition, the absolute configuration of compound 1 was determined by calculated ECD data.Results: One previously undescribed tetracyclic triterpenoid derivative, named as integracide L(1), 12aacetoxy-4,4-dimethyl-24-methylene-5a-cholesta-8,14-diene-2a,3β,11β-triol(2), 12a-acetoxy-4,4-dime thyl-24-methylene-5a-cholesta-8-momoene-2a,3β,11β-triol(3), 12a-acetoxy-4,4-dimethyl-24-methy lene-5a-cholesta-8,14-diene-3β,11β-triol(4), and 12a-acetoxy-4,4-dimethyl-24-methylene-5acholesta-8-momoene-3β,11β-triol(5) were isolated from F. sporotrichioide. Moreover, compound 1 was rare tetracyclic triterpenoid with single methyl replacement at C-4 position.Conclusion: Compound 1 was a new tetracyclic triterpenoid isolated from the endophytic fungus F.sporotrichioides. In addition, compound 2 could inhibit the growth of three different human cancer cells significantly. Compounds 3 and 5 were found to possess better cytotoxic activities on Hep G-2 cells than the other compounds, with IC50values of(2.8 ± 0.1) and(6.3 ± 0.3) μmol/L respectively.展开更多
基金support from the Research Council of University of Sistan and Baluchestan, Iran
文摘2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl chloride catalysts the reaction is limited to give only 1,8-dioxo-octahydroxanthenes 3a-k in very good yields.
基金Supported by the Central University Basic Scientific Research Fund of Hunan University (2009)the Key Scientific and Technological Project of Changsha, Hunan Province (No. 0901077-31)
文摘The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.
基金supported by the National Natural Science Foundation of China (No. 21101097)Natural Science Foundation of Shandong Province (ZR2010BQ023)the State Key Laboratory of Solid Lubrication (No. 0701)
文摘Solvothermal reactions of 3,5-dimethyl-2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl) pyridine (L), 1,4-benzendicarboxylic acid (H2bdc), and transitional metal cations of M11 (M = Mn, Co, Cd) in the presence of oxalic acid (H2ox) afford three novel supramolecular polymers (CPs), namely, {[M2(ox)(L)2][bdc][M2(Hox)2(OH)(H2O)4]·3H2O}n (M = Mn for 1, Co for 2, Cd for 3). Single-crystal X-ray diffraction analysis reveals that complexes 1-3 are isostructural and the 3D supramolecular structure was connected through non-covalent interactions. With the help of H2ox, the L ligands cheated with center atoms forming a butterfly [M2(ox)(L)2]2+ building block. The bdc2- ligand linked with the unprecedented [M2(Hox)2(OH)2(H2O)4] units through strong O-H...O hydrogen bonds forming a zigzag chain, which are further connected through π-π interactions between L and bdc2- ligands to form a 3D supramolecular structure. Moreover, elemental analyses, IR, thermogravimetric, PXRD and luminescence have been investigated.
基金the Science Research Foundation of Henan Institute of Science and Technology (No. 06036)
文摘The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6)A, α = 112.566(1), β = 92.324(2), γ = 102.91(1)°, V= 1315.65(10) A^3, Z = 2, Dc = 1.344 g/cm^3,μ(MoKa) = 0.282 mm^-1, λ = 0.71073 A, F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C( 12)-H(12)…O(1) and C(28)-H(28)...O(1)# 1 hydrogen bonds were observed in the title compound.
文摘The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkaline hydrolysis and nitrosation reactions. The yield of DMNNDO was increased from 37% to 45%. The structure of DMNNDO was characterized by IR,^1H NMR,^13 C NMR,and elemental analysis. Also the thermal decomposition of DMNNDO was studied by using DSC and TG-DTG to find that there are primarily two exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists as a dimeric form due to the presence of nitroso group. The crystal belongs to monoclinic system,space group C2/c with a = 14.515(3),b = 9.955(2),c = 11.897(2) °,β = 98.500(3)°,V = 1.6998(2) nm^3,Z = 8,D_c = 1.486 g×cm^-3,μ = 0.128 mm^-1,F(000) = 800,S = 1.055,R = 0.0358 and wR = 0.0917. In particular,DMNNDO could be easily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl_3 was revealed by means of NMR monitoring.
文摘Dimethyl-1-(1, 2, 4-triazol) -2- butanone was treated with aqueous formaldehyde to give an additional product, and subsequent elimination by acetic anhydride yielded 4, 4-dimethyl-2-(1, 2, 4-triazol)-1-penten-3-one. Further addition with substituted amines provided a series of (1, 2, 4-triazol)-4, 4-dimethyl-3-pentanone, which were then reduced by KBH4 to obtain a series of (1, 2, 4-triazol)-4, 4-dimethyl-3-pentanol. Their structures were confirmed by 1HNMR and elemental analysis. The results of bioassay showed that the title products possess good fungicidal activities.
基金supported by the National Natural Science Foundation of China (No.20872057)
文摘Three new crystalline compounds 1-3 were successfully obtained by the reactions of 3,3'-dimethoxy-6,6'-dimethyl-2,2'-bipyridine ligand(dmbp) with the corresponding Cu(Ⅰ) salts.Crystal data for 1:orthorhombic Pbca,a = 18.5858(12),b = 8.1821(5),c = 20.6066(13) ,V = 3133.7(3) 3,Z = 8,Dc = 1.843 g/cm3,F(000) = 1696,μ = 3.366 mm-1,the final R = 0.0223 and wR = 0.0542.Crystal data for 2:Orthorhombic Pbca,a = 18.7883(16),b = 8.3249(7),c = 19.0294(17) ,V = 2976.4(4) 3,Z = 8,Dc = 1.731 g/cm3,F(000) = 1552,μ = 4.154 mm-1,the final R = 0.0279 and wR = 0.0680.Crystal data for 3:monoclinic P21/c,a = 13.812(10),b = 9.910(7),c = 23.444(17) ,β = 104.3350(10)°,V = 3090(4) 3,Z = 4,Dc = 1.476 g/cm3,F(000) = 1408,μ = 1.588 mm-1,the final R = 0.0479 and wR = 0.1081.The results of X-ray crystallographic analysis revealed that C14H16ICuN2O2(1) and C14H16BrCuN2O2(2) are isostructural compounds with the dimers connected by C-H···halogen hydrogen bonds to generate a three-dimensional(3D) supramolecular network in 1 and a two-dimensional(2D) sheet structure in 2,respectively,while the mononuclear complex C28H32Cl2Cu2N4O4(3) is ionic.In 3,the [Cu(dmbp)2]+ cations and [ClCuCl]-anions are connected by C-H···Cl hydrogen bonds to form a one-dimensional(1D) chain along the a axis.Therefore,in the three complexes,the C-H···halogen hydrogen bonds dominate their crystal structures.Additionally,The UV luminescent properties of complexes 1-3 were investigated.
基金Supported by the National Natural Science Foundation of China( No. 2 9872 0 12)
文摘Started from 5-hydroxy-2-pentanone, (R)(E)-3,7-dimethyl-2-octene-1,8-dioic acid, callosobruchusic acid, was synthesized via five steps with D-(-)-camphor sultam as the chiral auxiliary. It was of good optical purity and yield.
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.
基金Project supported by the National Natural Science Foundation of China(No.21442014)
文摘The title compound, (E)-1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)- 3-(2-methoxyphenyl)-2-(1H-1,2,4-triazol-1-yl)propenol (3a), was synthesized by the Aldol con- densation reaction of 1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)-2-(1,2,4-triazol- 1-yl)ethanone with 2-methoxybenzaldehyde and then reduced with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction: monoclinic system, space group P21 with a = 6.2002(3), b = 12.8452(7), c = 13.2257(7) ?, Z = 2, V = 1031.23(9) ?3, Mr = 407.46, Dc = 1.312 Mg/m3, S = 1.054, μ = 0.091 mm-1, F(000) = 432, the final R = 0.0353 and wR = 0.0769 for 3161 observed reflections (I 〉 2σ(I)). X-ray analysis displays that the title compound adopts an E configuration for the C(7)=C(8) double bond and S configuration for the chirality center with the specific rotation of –63.75°. Furthermore, the stability of the crystal was maintained through the intermolecular hydrogen bond O(1)–H???N(3). The antitumor assay exhibits that the title compound 3a (E configuration) has a good antitumor activity against the Hela cell line with the IC50 value of 36.9 μM, which is better than that of 3b (Z configuration).
基金This work was supported by the Phytochemistry Key Laboratory of Shaanxi Province (No. 02js40)
文摘The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150(3), b = 9.906(3), c = 13.624(4) A, β = 106.360(4)°, V= 1443.9(7) ,A^3, Z = 4, Dc = 1.294 g/cm^3, F(000) = 592,μ(MoKa) = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O(2)-C(10) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0026 A) with the dihedral angle between them of 6.3°.
基金The authors are grateful for the financial support of the National Natural Science Foundation of China (No. 20104005).
文摘Novel polycarbonates from 5-allyloxy-1, 3-dioxan-2-one (ATMC) with 5, 5-dimethyl- 1, 3-dioxan-2-one (DTC) were successfully synthesized for the first time using immobilized porcine pancreas lipase (IPPL) as catalyst. The resulting copolymers were characterized by IR, ^1H NMR, ^13C NMR and GPC. The molecular weight (Mn) of the copolymer with molar feed ratio of 10:90 (ATMC:DTC) was 9300 and the polydispersity was 1.31, while the Mn increased to 14300 and polydispersity of 1.25 with the feed ratio of 50:50. Moreover, the composition of the copolymers agreed well with the monomer feed.
文摘从草苁蓉75%乙醇提取物中分离得到了2个单萜苷类化合物,结合其理化性质,并通过1DNMR(1 H NMR,13 C NMR)及1 H-1 H COSY、HSQC、HMBC、NOESY等多种波谱学方法进行结构鉴定,鉴定2个化合物分别为β-D-glucopyranose 1-(3,7-dimethyl-2-trans-6-octa-dienoate)(化合物1)和6,7-dihydrofoliamenthoic acid diglucoside(化合物2),其中化合物1为新化合物,化合物2为第1次从列当科植物中获得.
基金supported by the International S&T Cooperation Program of China(No.2015DFG92750)the National Natural Science Foundation of China(Nos.51478172 and 51278464)the Natural Science Foundation of Zhejiang Province of China(No.LY17E080002)
文摘In this study,the performance of 3,5-dimethyl-2,4-dichlorophenol(DCMX) degradation by a screened strain was investigated.18 S r DNA and the neighbor-joining method were used for identification of the isolated strain.The results of phylogenetic analysis and scanning electron micrographs showed that the most probable identity of the screened strain should be Penicillium sp.Growth characteristics of Penicillium sp.and degradation processes of DCMX were examined.Fourier transform infrared spectroscopy of the inoculated DCMX solution was recorded,which supported the capacity of DCMX degradation by the screened Penicillium sp.Under different salinity conditions,the highest growth rate and removal efficiency for DCMX were obtained at p H 6.0.The removal efficiency decreased from 100%to 66% when the DCMX concentration increased from 5 to 60 mg/L,respectively.Using a Box–Behnken design,the maximum DCMX removal efficiency was determined to be 98.4%.With acclimation to salinity,higher removal efficiency could be achieved.The results demonstrate that the screened Penicillium sp.has the capability for degradation of DCMX.
文摘A combination of HBr and trans-3,5-dihydroperoxy-3,5-dimethyl-1,2-dioxolane as anew and powerful oxidant was found effective for facile brotnination of different aromatic compounds at room temperature in water as a green solvent.Mild reaction conditions,high selectivity and yield,high reaction rate and non-toxicity are some of the major advantages of this synthetic protocol.
基金Project supported by the National Natural Science Foundation of China.
文摘Compact and high reliable blue coherent light sources are required for the optical data storage of high density, color image processing and optical measurements.One of the possible approaches is the direct frequency doubling of the near infrared semiconductor laser by optical waveguide techniques. So a material applied to the second harmonic generation (SHG) must not only have high molecular hyperpolarizability (β) but also have complete transparency at both the
文摘Two novel constituents were isolated from the roots of Chinese medicinal herbs, Salvia miltiorrhiza. Their structures were determined by spectroscopic technique. The compounds were named 13,14-dihydroxy-15-methyl-benzo[2,3-a]-7,7-dimethyl-12-oxa-tricyclo[4,4,21.4,0]dodecane(1) and 16-methyl-tropono[2,3-c]-7,7-dimethyl-12-oxa-tricyclo[4,4,21.4,0]dodecane(2).
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.
基金funded by Outstanding Youth Foundation of Heilongjiang province(NO.YQ2021H009).
文摘Objective: To isolate bioactive compounds from the endophytic fungus Fusarium sporotrichioides isolated from Rauwolfia yunnanensis, and investigate their pharmacological activities.Methods: The chemical constituents were isolated and purified by combining with ODS column chromatography, silica gel column chromatography and by performing semipreparative HPLC. Their structures were established on the basis of 1D NMR(1H-NMR and13C-NMR) and 2D NMR(1H–1H COSY,HSQC, HMBC and NOESY), as well as HRESIMS and comparison with literature data. In addition, the absolute configuration of compound 1 was determined by calculated ECD data.Results: One previously undescribed tetracyclic triterpenoid derivative, named as integracide L(1), 12aacetoxy-4,4-dimethyl-24-methylene-5a-cholesta-8,14-diene-2a,3β,11β-triol(2), 12a-acetoxy-4,4-dime thyl-24-methylene-5a-cholesta-8-momoene-2a,3β,11β-triol(3), 12a-acetoxy-4,4-dimethyl-24-methy lene-5a-cholesta-8,14-diene-3β,11β-triol(4), and 12a-acetoxy-4,4-dimethyl-24-methylene-5acholesta-8-momoene-3β,11β-triol(5) were isolated from F. sporotrichioide. Moreover, compound 1 was rare tetracyclic triterpenoid with single methyl replacement at C-4 position.Conclusion: Compound 1 was a new tetracyclic triterpenoid isolated from the endophytic fungus F.sporotrichioides. In addition, compound 2 could inhibit the growth of three different human cancer cells significantly. Compounds 3 and 5 were found to possess better cytotoxic activities on Hep G-2 cells than the other compounds, with IC50values of(2.8 ± 0.1) and(6.3 ± 0.3) μmol/L respectively.