A new phloretin derivative 1 3-[2-(4-hydroxy-phenyl)-ethyl]-benzo[d] isoxazole-4,6-diol (yield 63%) was synthesized from phloretin by carbonyl nucleophilic addition condensation reaction. Its structure was characteriz...A new phloretin derivative 1 3-[2-(4-hydroxy-phenyl)-ethyl]-benzo[d] isoxazole-4,6-diol (yield 63%) was synthesized from phloretin by carbonyl nucleophilic addition condensation reaction. Its structure was characterized by 1H NMR, 13C NMR and HR-MS. The phloretin, compound 1, resveratrol and acetylated resveratrol were determined by comparing them with paclitaxel. Anti-tumor activity of alcohol on SPC-A1, EC109, A549, MCF-7 and MDA-MB-231 cell lines. Compound 1 showed better antitumor activity than docetaxel against A549 tumor cells.展开更多
A series of iron-based Fischer-Tropsch synthesis (FTS) catalysts incorporated with Al2O3 binder were prepared by the combination of co-precipitation and spray drying technology. The catalyst samples were characteriz...A series of iron-based Fischer-Tropsch synthesis (FTS) catalysts incorporated with Al2O3 binder were prepared by the combination of co-precipitation and spray drying technology. The catalyst samples were characterized by using N2 physical adsorption, temperature-programmed reduction/desorption (TPR/TPD) and MSssbauer effect spectroscopy (MES) methods. The characterization results indicated that the BET surface area increases with increasing Al2O3 content and passes through a maximum at the Al2O3/Fe ratio of 10/100 (weight basis). After the point, it decreases with further increase in Al2O3 content. The incorporation of Al2O3 binder was found to weaken the surface basicity and suppress the reduction and carburization of iron-based catalysts probably due to the strong K-Al2O3 and Fe-Al2O3 interactions. Furthermore, the H2 adsorption ability of the catalysts is enhanced with increasing Al2O3 content. The FTS performances of the catalysts were tested in a slurry-phase continuously stirred tank reactor (CSTR) under the reaction conditions of 260 ℃, 1.5 MPa, 1000 h^-1 and molar ratio of H2/CO 0.67 for 200 h. The results showed that the addition of small amounts of Al2O3 affects the activity of iron-based catalysts to a little extent. However, with further increase of Al2O3 content, the FTS activity and water gas shift reaction (WGS) activity are decreased severely. The addition of appropriate Al2O3 do not affect the product selectivity, but the catalysts incorporated with large amounts of Al2O3 have higher selectivity for light hydrocarbons and lower selectivity for heavy hydrocarbons.展开更多
LiMn2O4 spinel cathode materials were modified with 2 wt.%Li-M-PO4(M=Co,Ni,Mn) by polyol synthesis method.The phosphate surface-modified LiMn2O4 cathode materials were physically characterized by X-ray diffraction(...LiMn2O4 spinel cathode materials were modified with 2 wt.%Li-M-PO4(M=Co,Ni,Mn) by polyol synthesis method.The phosphate surface-modified LiMn2O4 cathode materials were physically characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM) and energy dispersive X-ray spectroscopy(EDS).The charge-discharge test showed that the cycling and rate capacities of LiMn2O4 cathode materials were significantly enhanced by stabilizing the electrode surface with phosphate.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
Al2O3-metal composite coatings with different reactants and diluents were fabricated on mild steel plate with nonpressure combustion synthesis process. The coat-ings were characterized by means of X-ray diffraction, s...Al2O3-metal composite coatings with different reactants and diluents were fabricated on mild steel plate with nonpressure combustion synthesis process. The coat-ings were characterized by means of X-ray diffraction, scanning electron microscopy, and energy-dispersive spec-trometry, respectively. Thermal shock tests were carried out to determine the bond strength of the coating with the steel substrate. The results indicate that the coating is composed of α-A1203, α-(Fe-Cr) and Al2SiO5 as the main phases. It is found that the coating with the diluents of Al2O3-SiO2 and transition layer of Al2O3-Cr presents the hi.ghest hardness of 2270 HV0.2 and the lowest porosity of 3.93 %. Owing to a metallurgical bond of the coating-to-substrate, the coating exhibits a good thermal shock resistance.展开更多
Methanol synthesis from hydrogenation of CO2 is investigated over Cu/ZnO/Al2O3 catalysts prepared by decomposition of M(Cu,Zn)-ammonia complexes (DMAC) at various temperatures.The catalysts were characterized in d...Methanol synthesis from hydrogenation of CO2 is investigated over Cu/ZnO/Al2O3 catalysts prepared by decomposition of M(Cu,Zn)-ammonia complexes (DMAC) at various temperatures.The catalysts were characterized in detail,including X-ray diffraction,N2 adsorption-desorption,N2O chemisorption,temperature-programmed reduction and evolved gas analyses.The influences of DMAC temperature,reaction temperature and specific Cu surface area on catalytic performance are investigated.It is considered that the aurichalcite phase in the precursor plays a key role in improving the physiochemical properties and activities of the final catalysts.The catalyst from rich-aurichalcite precursor exhibits large specific Cu surface area and high space time yield of methanol (212 g/(Lcat·h);T=513 K,p=3MPa,SV=12000 h-1).展开更多
2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol(C6H12N2O8) was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the t...2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol(C6H12N2O8) was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the title compound was characterized by 1H NMR,13C NMR,FT-IR,elementary analysis,and X-ray single-crystal diffraction analysis,which reveals that the title compound crystallizes in triclinic,space group P with a = 0.6324(2),b = 0.6454(3),c = 0.7062(3) nm,α= 111.550(4),β= 95.505(4),γ= 113.395(4)°,V = 0.23595(16) nm3,Z = 1,Mr = 240.18,Dc = 1.690 g·cm-3,μ = 0.159 mm-1,F(000) = 126,R = 0.0304 and wR = 0.0907.展开更多
Normal spinel LiMn 2O 4 was synthesized by sol-gel method using lithium nitrate,manganese nitrate,citric acid and ethylene glycol as raw materials. LiMn 2O 4 was characterized by XRD,TG-DTA,IR,SEM and AAS.The opti...Normal spinel LiMn 2O 4 was synthesized by sol-gel method using lithium nitrate,manganese nitrate,citric acid and ethylene glycol as raw materials. LiMn 2O 4 was characterized by XRD,TG-DTA,IR,SEM and AAS.The optimum conditions for the synthesis were explored.Citric acid and ethylene glycol were mixed with molar ratio of 0.25,and the mixture was esterified at 140℃ for 4 hours.Then lithium nitrate and manganese nitrate were added with molar ratio of 0.6. In the system,the total molar of cations was equal to that of citric acid. At last, reflux the system at 105℃ for 2 hours. Dried gel was fired at 600℃ for 8 hours. Particle diameters of raw product were about 100 nm mainly. Further research shows that lithium ion of LiMn 2O 4 is easy to be extracted,and normal spinel λ-MnO 2 can be obtained after lithium ion extraction.展开更多
The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-cr...The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5)A,β = 99.364(2) °,V = 4332.58(18) A^3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm^-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.展开更多
The title compound 2-(3-methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline- 1,3-dione (C12H10NaO2S, Mr= 274.30) has been synthesized by a three-step procedure including the cyclization, hydrazinolysis and s...The title compound 2-(3-methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline- 1,3-dione (C12H10NaO2S, Mr= 274.30) has been synthesized by a three-step procedure including the cyclization, hydrazinolysis and substitution reactions, and its crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2/c with a = 12.264(3), b = 14.646(3), c = 14.349(4) A,β = 91.69(3)°,μ = 0.255 mm1, Mr = 274.30, V = 2576.2(10) A3, Z =8, Dc = 1.414 g/cm3, F(000) = 1136, R = 0.0487 and wR = 0.1329 for 4048 observed reflections with I 〉 2σ(I). In addition, the preliminary bioassay suggested that the title compound 6 exhibits relatively good antitumor activity against HT-29 and MCF-7.展开更多
The title compound (E)-4-tert-butyl-N-(2,4-dichlorobenzylidene)-5-(1,2,4-triazol-1-yl)-thiazol-2-amine was synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-thiazol-2-amine with 2,4-dichlorobe...The title compound (E)-4-tert-butyl-N-(2,4-dichlorobenzylidene)-5-(1,2,4-triazol-1-yl)-thiazol-2-amine was synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-thiazol-2-amine with 2,4-dichlorobenzaldehyde, and its crystal structure was determined by singlecrystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9748(4), b = 10.1803(5), c = 11.4603(6), α = 102.882(1), β = 100.253(1), γ = 104.457(1)°, V = 850.95(7)3, Z = 2, F(000) = 392, C16H15Cl2N5S, Mr = 380.29, Dc = 1.484 g/cm3, S = 1.095, μ = 0.512 mm-1, the final R = 0.0301 and wR = 0.0965 for 3334 observed reflections (I 〉 2σ(I)). The preliminary antitumor activity shows that for the title compound the IC50 of Hela is 0.175 μmol/mL and that of Bel7402 is 0.156 μmol/mL.展开更多
The title compound was synthesized by the reaction of 4-tert-butyl-5-(4-chlorobenzyl)-2-aminothiazole with 2,6-difluorobenzoic acid. The crystal structure of the title compound, C21H19ClF2N2OS, was determined by sin...The title compound was synthesized by the reaction of 4-tert-butyl-5-(4-chlorobenzyl)-2-aminothiazole with 2,6-difluorobenzoic acid. The crystal structure of the title compound, C21H19ClF2N2OS, was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pbca with a = 12.6479(13), b = 13.1204(13), c = 14.1341(15), Z = 4, V = 2011.5(4)3, Mr = 420.89, Dc = 1.390 g/cm3, S = 1.023, μ = 0.326 mm-1, F(000) = 872, the final R = 0.0365 and wR = 0.0880 for 6101 observed reflections(I 〉 2σ(I)), and R = 0.0507, wR = 0.0978 for 7779 independent reflections. X-ray crystal structure displays that the hydrogen bonding interactions observed link the molecules to form a dimeric unit. The preliminary biological test of the title compound shows good antitumor activity, with IC50 of 0.046 μmol/mL against the Hela cell line.展开更多
The title compound has been synthesized by the reaction of 4-tert-butyl-5-(1,2,4- triazol-1-yl)-2-aminothiazole with propionic anhydride, and its crystal structure was determined by single-crystal X-ray diffraction....The title compound has been synthesized by the reaction of 4-tert-butyl-5-(1,2,4- triazol-1-yl)-2-aminothiazole with propionic anhydride, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbca with α = 18.441(2), b = 8.3284(9), c = 19.257(2) A, Z = 8, V = 2957.5(5) A3, Mr = 279.37, Dc = 1.255 mg/m3, S = 1.033, μ =0.219 mm^-1, F(000) = 1184, the final R = 0.0349 and wR = 0.0876 for 2629 observed reflections (I 〉 2σ(I)). X-ray crystal structure presents the intermolecular N–H···N hydrogen bond, which plays an important role in stabilizing the crystal structure. The preliminary bioassay indicates that the title compound exhibits potent fungicidal activity against R. Solani (25 mg/L) with inhibition rate of 80.0%.展开更多
The title compound (E)-2-[(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crys...The title compound (E)-2-[(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 5.9362(8), b = 11.5070(15), c = 29.460(4)A, β= 97.326(3)°, V = 1995.9(5) A^3, Z = 4, F(000) = 808, C22H24N2O2S, Mr= 380.49, De= 1.266 g/cm^3, S = 1.031,μ = 0.181 mm^-1, the final R = 0.0474 and wR = 0.1441 for 4327 observed reflections (I 〉 2σ(I)). Intramolecular O-H…N hydrogen bond is observed in the crystal. The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.展开更多
Co-Ni/Al2O3catalyst was prepared by the fusion method and used in Fischer-Tropsch synthesis(FTS).The catalysts were characterized by means of nitrogen sorption and scanning electron microscopy.The effect of some react...Co-Ni/Al2O3catalyst was prepared by the fusion method and used in Fischer-Tropsch synthesis(FTS).The catalysts were characterized by means of nitrogen sorption and scanning electron microscopy.The effect of some reaction conditions such as temperature,pressure and H2/CO feed ratio on the catalytic performance of Co-Ni/Al2O3in CO hydrogenation was investigated in a fixed-bed reactor.The results indicate that the optimum reaction conditions are 250℃,0.3 MPa,H2/CO feed ratio of 2.0,and GHSV of 3 000 h-1.Kinetically,the reaction rate was correlated with the Langmuir-Hinshelwood-Hougen-Watson type models.The activation energy for the best fitted model is 88.41 kJ/mol,suggesting that the intra-particle mass transport is not significant.展开更多
Fifteen novel 2-(3-oxobenzo[d]isothiazol-2(3H)-yl)ethyl benzoates were synthesi- zed by the condensation of 2-(2-hydroxyethyl)benzo[d]isothiazol-3(2H)-one with substituted benzoic acids in dichloromethane. All...Fifteen novel 2-(3-oxobenzo[d]isothiazol-2(3H)-yl)ethyl benzoates were synthesi- zed by the condensation of 2-(2-hydroxyethyl)benzo[d]isothiazol-3(2H)-one with substituted benzoic acids in dichloromethane. All the compounds were characterized by elemental analysis, IR, ESI-MS and 1H NMR. The crystal structures for 2-(2-hydroxyethyl)benzo[d]isothiazol-3(2H)-one (2) and 2-(3-oxobenzo[d]isothiazol-2(3H)-yl)ethyl 2-methoxybenzoate (30) have been determined by X-ray crystal structure analysis. Compound 2 (C9H9NO2S) crystallizes in the monoclinic system, space group Pn with a = 10.552(3), b = 7.849(2), c = 10.765(4) A, β = 103.128(4)°, V= 868.3(5) A3, Mr = 195.24, Dc = 1.493 Mg.m-3, μ = 0.33 mm-1, F(000) = 408, Z = 4, R= 0.0314 and wR= 0.0628. Compound 30 (C17H15NO4S) crystallizes in the triclinic system, space group P1 with a = 8.028(2), b = 9.300(2), c = 10.430(3)A, V= 752.1(3)A3, Mr = 329.36, D,= 1.454 Mg.m-3, p = 0.24 mm-1, F(000) = 344, Z = 2, R = 0.0377 and wR = 0.0904. The preliminary biological test indicated that the title compounds show better growth inhibitory activity against the gram-positive bacteria than the gram-negative bacteria.展开更多
5,7-Dimethoxy-2-phenylquinolin-4-yl phenyloxy (N-L-alanine ethyl ester) phosphoramidate (C28H29N2O7P, Mr = 536.17) has been synthesized by a facial phosphorylated reaction, and its structure was determined by IR, ...5,7-Dimethoxy-2-phenylquinolin-4-yl phenyloxy (N-L-alanine ethyl ester) phosphoramidate (C28H29N2O7P, Mr = 536.17) has been synthesized by a facial phosphorylated reaction, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^-, with a = 11.375(2), b = 11.591(2), c = 11.638(2) A^°, α= 109.46(3), β= 104.58(3), γ= 100.48(3)°, V = 1339.6(5)A^°^3, Z = 2, Dc = 1.330 g/cm^3,μ = 0.152 mm^-1, F(000) = 564, the final R = 0.0654 and wR = 0.1546. In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking diastereoisomers. The compound has a noteworthy feature in the framework, and such units are linked by two equal intermolecular P=O…H-N hydrogen bonds.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 title compound N-((3-(2-nitrophenyl) propanoyl)oxy)-N-phenylbenzamide(C22H18N2O5,Mr = 390.38) was synthesized with nitrobenzene as the starting materials and structurally characterized by 1H NMR,13 C NMR,I...The title compound N-((3-(2-nitrophenyl) propanoyl)oxy)-N-phenylbenzamide(C22H18N2O5,Mr = 390.38) was synthesized with nitrobenzene as the starting materials and structurally characterized by 1H NMR,13 C NMR,IR,H RMS(E-SI) and single-crystal X-ray diffraction.The crystalline structure of the title compound was studied in detail.The single-crystal X-ray diffraction revealed that the compound crystallizes in monoclinic,space group P21/n,with a = 14.4481(7),b = 8.0089(5),c = 16.6808(9) A,α = 90.00(5),β = 100.069(5),γ = 90.00(5)°,Mr = 390.38,V = 1900.46(18) A^3,Z = 4,Dc = 1.364 g/cm^-3,μ = 0.098,F(000) = 816.0,the final R = 0.0530 and w R = 0.1141 for 2525 observed reflections(I 〉 2σ(I)),R(all data) = 0.0813,w R(all data) = 0.1335,completeness to theta of 26.020 is 99.8% and GOF = 1.085.The crystal structure contains three branched chains with its center placed at the midpoint of N.The phenyl ring(C(8)~C(13)) makes a dihedral angle of 83.5(1) ℃ with the phenyl ring(C(1)~C(6)),and 80.5(1) ℃with the nitro-substituted benzene ring(C(17)~C(22)),indicating that the three rings are not coplanar.Hydrogen bonds(C(10)–H(10)···O(3)),(C(15)–H(15B)···O(4) and C(16)–H(16B)···O(4)) together with π-π stacking interactions stabilize the structure of the molecule.The preliminary biological test shows that the title compound has good antitumor activity against A549 in vitro with the IC50 value of 3.17 μmol.展开更多
文摘A new phloretin derivative 1 3-[2-(4-hydroxy-phenyl)-ethyl]-benzo[d] isoxazole-4,6-diol (yield 63%) was synthesized from phloretin by carbonyl nucleophilic addition condensation reaction. Its structure was characterized by 1H NMR, 13C NMR and HR-MS. The phloretin, compound 1, resveratrol and acetylated resveratrol were determined by comparing them with paclitaxel. Anti-tumor activity of alcohol on SPC-A1, EC109, A549, MCF-7 and MDA-MB-231 cell lines. Compound 1 showed better antitumor activity than docetaxel against A549 tumor cells.
基金The financial support from the National Natural Science Foundation of China (20590361)the National Outstanding Young Scientists Foundation of China (20625620)
文摘A series of iron-based Fischer-Tropsch synthesis (FTS) catalysts incorporated with Al2O3 binder were prepared by the combination of co-precipitation and spray drying technology. The catalyst samples were characterized by using N2 physical adsorption, temperature-programmed reduction/desorption (TPR/TPD) and MSssbauer effect spectroscopy (MES) methods. The characterization results indicated that the BET surface area increases with increasing Al2O3 content and passes through a maximum at the Al2O3/Fe ratio of 10/100 (weight basis). After the point, it decreases with further increase in Al2O3 content. The incorporation of Al2O3 binder was found to weaken the surface basicity and suppress the reduction and carburization of iron-based catalysts probably due to the strong K-Al2O3 and Fe-Al2O3 interactions. Furthermore, the H2 adsorption ability of the catalysts is enhanced with increasing Al2O3 content. The FTS performances of the catalysts were tested in a slurry-phase continuously stirred tank reactor (CSTR) under the reaction conditions of 260 ℃, 1.5 MPa, 1000 h^-1 and molar ratio of H2/CO 0.67 for 200 h. The results showed that the addition of small amounts of Al2O3 affects the activity of iron-based catalysts to a little extent. However, with further increase of Al2O3 content, the FTS activity and water gas shift reaction (WGS) activity are decreased severely. The addition of appropriate Al2O3 do not affect the product selectivity, but the catalysts incorporated with large amounts of Al2O3 have higher selectivity for light hydrocarbons and lower selectivity for heavy hydrocarbons.
基金financially supported by the National High-Tech Research and Development(863) Program of China(No.2006AA11A160)the National Natural Science Foundation of China(No.50604018)
文摘LiMn2O4 spinel cathode materials were modified with 2 wt.%Li-M-PO4(M=Co,Ni,Mn) by polyol synthesis method.The phosphate surface-modified LiMn2O4 cathode materials were physically characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM) and energy dispersive X-ray spectroscopy(EDS).The charge-discharge test showed that the cycling and rate capacities of LiMn2O4 cathode materials were significantly enhanced by stabilizing the electrode surface with phosphate.
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financially supported by the Ministry of Education of China(No.625010312)
文摘Al2O3-metal composite coatings with different reactants and diluents were fabricated on mild steel plate with nonpressure combustion synthesis process. The coat-ings were characterized by means of X-ray diffraction, scanning electron microscopy, and energy-dispersive spec-trometry, respectively. Thermal shock tests were carried out to determine the bond strength of the coating with the steel substrate. The results indicate that the coating is composed of α-A1203, α-(Fe-Cr) and Al2SiO5 as the main phases. It is found that the coating with the diluents of Al2O3-SiO2 and transition layer of Al2O3-Cr presents the hi.ghest hardness of 2270 HV0.2 and the lowest porosity of 3.93 %. Owing to a metallurgical bond of the coating-to-substrate, the coating exhibits a good thermal shock resistance.
基金supported by the National Basic Research Program of China (No. 2011CB201404)the financial support of the State Key Laboratory for Oxo Synthesis and Selective Oxidation (OSSO) of China
文摘Methanol synthesis from hydrogenation of CO2 is investigated over Cu/ZnO/Al2O3 catalysts prepared by decomposition of M(Cu,Zn)-ammonia complexes (DMAC) at various temperatures.The catalysts were characterized in detail,including X-ray diffraction,N2 adsorption-desorption,N2O chemisorption,temperature-programmed reduction and evolved gas analyses.The influences of DMAC temperature,reaction temperature and specific Cu surface area on catalytic performance are investigated.It is considered that the aurichalcite phase in the precursor plays a key role in improving the physiochemical properties and activities of the final catalysts.The catalyst from rich-aurichalcite precursor exhibits large specific Cu surface area and high space time yield of methanol (212 g/(Lcat·h);T=513 K,p=3MPa,SV=12000 h-1).
基金Supported by the National "973" project (No. 613740102)
文摘2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol(C6H12N2O8) was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the title compound was characterized by 1H NMR,13C NMR,FT-IR,elementary analysis,and X-ray single-crystal diffraction analysis,which reveals that the title compound crystallizes in triclinic,space group P with a = 0.6324(2),b = 0.6454(3),c = 0.7062(3) nm,α= 111.550(4),β= 95.505(4),γ= 113.395(4)°,V = 0.23595(16) nm3,Z = 1,Mr = 240.18,Dc = 1.690 g·cm-3,μ = 0.159 mm-1,F(000) = 126,R = 0.0304 and wR = 0.0907.
基金FundedbytheNationalNaturalScienceFoundationofChi na (No .5 9972 0 2 7)
文摘Normal spinel LiMn 2O 4 was synthesized by sol-gel method using lithium nitrate,manganese nitrate,citric acid and ethylene glycol as raw materials. LiMn 2O 4 was characterized by XRD,TG-DTA,IR,SEM and AAS.The optimum conditions for the synthesis were explored.Citric acid and ethylene glycol were mixed with molar ratio of 0.25,and the mixture was esterified at 140℃ for 4 hours.Then lithium nitrate and manganese nitrate were added with molar ratio of 0.6. In the system,the total molar of cations was equal to that of citric acid. At last, reflux the system at 105℃ for 2 hours. Dried gel was fired at 600℃ for 8 hours. Particle diameters of raw product were about 100 nm mainly. Further research shows that lithium ion of LiMn 2O 4 is easy to be extracted,and normal spinel λ-MnO 2 can be obtained after lithium ion extraction.
基金Supported by the Natural Science Foundation of Hubei Province (2006ABB016)Key Science Research Project of Hubei Provincial Department of Education (No.D200724001)the Science Research Project of Yunyang Medical College (No.2008CXG01)
文摘The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5)A,β = 99.364(2) °,V = 4332.58(18) A^3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm^-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.
基金supported by the National Natural Science Foundation of China(21102069 and 21372113)the Project of Science and Technology New Star in Zhujiang Guangzhou city(No.2012J2200051)
文摘The title compound 2-(3-methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline- 1,3-dione (C12H10NaO2S, Mr= 274.30) has been synthesized by a three-step procedure including the cyclization, hydrazinolysis and substitution reactions, and its crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2/c with a = 12.264(3), b = 14.646(3), c = 14.349(4) A,β = 91.69(3)°,μ = 0.255 mm1, Mr = 274.30, V = 2576.2(10) A3, Z =8, Dc = 1.414 g/cm3, F(000) = 1136, R = 0.0487 and wR = 0.1329 for 4048 observed reflections with I 〉 2σ(I). In addition, the preliminary bioassay suggested that the title compound 6 exhibits relatively good antitumor activity against HT-29 and MCF-7.
基金Supported by the Natural Science Foundation of Hunan Province (No. 07JJ302)
文摘The title compound (E)-4-tert-butyl-N-(2,4-dichlorobenzylidene)-5-(1,2,4-triazol-1-yl)-thiazol-2-amine was synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-thiazol-2-amine with 2,4-dichlorobenzaldehyde, and its crystal structure was determined by singlecrystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9748(4), b = 10.1803(5), c = 11.4603(6), α = 102.882(1), β = 100.253(1), γ = 104.457(1)°, V = 850.95(7)3, Z = 2, F(000) = 392, C16H15Cl2N5S, Mr = 380.29, Dc = 1.484 g/cm3, S = 1.095, μ = 0.512 mm-1, the final R = 0.0301 and wR = 0.0965 for 3334 observed reflections (I 〉 2σ(I)). The preliminary antitumor activity shows that for the title compound the IC50 of Hela is 0.175 μmol/mL and that of Bel7402 is 0.156 μmol/mL.
基金Project supported by the National Technology R&D Program(No.2011 BAE06B01)
文摘The title compound was synthesized by the reaction of 4-tert-butyl-5-(4-chlorobenzyl)-2-aminothiazole with 2,6-difluorobenzoic acid. The crystal structure of the title compound, C21H19ClF2N2OS, was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pbca with a = 12.6479(13), b = 13.1204(13), c = 14.1341(15), Z = 4, V = 2011.5(4)3, Mr = 420.89, Dc = 1.390 g/cm3, S = 1.023, μ = 0.326 mm-1, F(000) = 872, the final R = 0.0365 and wR = 0.0880 for 6101 observed reflections(I 〉 2σ(I)), and R = 0.0507, wR = 0.0978 for 7779 independent reflections. X-ray crystal structure displays that the hydrogen bonding interactions observed link the molecules to form a dimeric unit. The preliminary biological test of the title compound shows good antitumor activity, with IC50 of 0.046 μmol/mL against the Hela cell line.
基金supported by the Natural Science Foundation of Hunan Province(No.12jj3012)
文摘The title compound has been synthesized by the reaction of 4-tert-butyl-5-(1,2,4- triazol-1-yl)-2-aminothiazole with propionic anhydride, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbca with α = 18.441(2), b = 8.3284(9), c = 19.257(2) A, Z = 8, V = 2957.5(5) A3, Mr = 279.37, Dc = 1.255 mg/m3, S = 1.033, μ =0.219 mm^-1, F(000) = 1184, the final R = 0.0349 and wR = 0.0876 for 2629 observed reflections (I 〉 2σ(I)). X-ray crystal structure presents the intermolecular N–H···N hydrogen bond, which plays an important role in stabilizing the crystal structure. The preliminary bioassay indicates that the title compound exhibits potent fungicidal activity against R. Solani (25 mg/L) with inhibition rate of 80.0%.
基金the National Project of Scientific and Technical Supporting Programs and Ministry of Science & Technology of China (No.2006BAE01A01-4)
文摘The title compound (E)-2-[(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 5.9362(8), b = 11.5070(15), c = 29.460(4)A, β= 97.326(3)°, V = 1995.9(5) A^3, Z = 4, F(000) = 808, C22H24N2O2S, Mr= 380.49, De= 1.266 g/cm^3, S = 1.031,μ = 0.181 mm^-1, the final R = 0.0474 and wR = 0.1441 for 4327 observed reflections (I 〉 2σ(I)). Intramolecular O-H…N hydrogen bond is observed in the crystal. The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.
文摘Co-Ni/Al2O3catalyst was prepared by the fusion method and used in Fischer-Tropsch synthesis(FTS).The catalysts were characterized by means of nitrogen sorption and scanning electron microscopy.The effect of some reaction conditions such as temperature,pressure and H2/CO feed ratio on the catalytic performance of Co-Ni/Al2O3in CO hydrogenation was investigated in a fixed-bed reactor.The results indicate that the optimum reaction conditions are 250℃,0.3 MPa,H2/CO feed ratio of 2.0,and GHSV of 3 000 h-1.Kinetically,the reaction rate was correlated with the Langmuir-Hinshelwood-Hougen-Watson type models.The activation energy for the best fitted model is 88.41 kJ/mol,suggesting that the intra-particle mass transport is not significant.
基金Supported by the National Natural Science Foundation of China (No. 20962007)
文摘Fifteen novel 2-(3-oxobenzo[d]isothiazol-2(3H)-yl)ethyl benzoates were synthesi- zed by the condensation of 2-(2-hydroxyethyl)benzo[d]isothiazol-3(2H)-one with substituted benzoic acids in dichloromethane. All the compounds were characterized by elemental analysis, IR, ESI-MS and 1H NMR. The crystal structures for 2-(2-hydroxyethyl)benzo[d]isothiazol-3(2H)-one (2) and 2-(3-oxobenzo[d]isothiazol-2(3H)-yl)ethyl 2-methoxybenzoate (30) have been determined by X-ray crystal structure analysis. Compound 2 (C9H9NO2S) crystallizes in the monoclinic system, space group Pn with a = 10.552(3), b = 7.849(2), c = 10.765(4) A, β = 103.128(4)°, V= 868.3(5) A3, Mr = 195.24, Dc = 1.493 Mg.m-3, μ = 0.33 mm-1, F(000) = 408, Z = 4, R= 0.0314 and wR= 0.0628. Compound 30 (C17H15NO4S) crystallizes in the triclinic system, space group P1 with a = 8.028(2), b = 9.300(2), c = 10.430(3)A, V= 752.1(3)A3, Mr = 329.36, D,= 1.454 Mg.m-3, p = 0.24 mm-1, F(000) = 344, Z = 2, R = 0.0377 and wR = 0.0904. The preliminary biological test indicated that the title compounds show better growth inhibitory activity against the gram-positive bacteria than the gram-negative bacteria.
基金supported by the National Natural Science Foundation of China (No. 20472076, 20572061, 20732004)Henan Academic Foundation of Science and Technology (No. 0512001400)
文摘5,7-Dimethoxy-2-phenylquinolin-4-yl phenyloxy (N-L-alanine ethyl ester) phosphoramidate (C28H29N2O7P, Mr = 536.17) has been synthesized by a facial phosphorylated reaction, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^-, with a = 11.375(2), b = 11.591(2), c = 11.638(2) A^°, α= 109.46(3), β= 104.58(3), γ= 100.48(3)°, V = 1339.6(5)A^°^3, Z = 2, Dc = 1.330 g/cm^3,μ = 0.152 mm^-1, F(000) = 564, the final R = 0.0654 and wR = 0.1546. In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking diastereoisomers. The compound has a noteworthy feature in the framework, and such units are linked by two equal intermolecular P=O…H-N hydrogen bonds.
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.
基金Supported by the Lanzhou Science and Technology Bureau Program Funds(2013-4-79,2014-1-174,2014-1-214)
文摘The title compound N-((3-(2-nitrophenyl) propanoyl)oxy)-N-phenylbenzamide(C22H18N2O5,Mr = 390.38) was synthesized with nitrobenzene as the starting materials and structurally characterized by 1H NMR,13 C NMR,IR,H RMS(E-SI) and single-crystal X-ray diffraction.The crystalline structure of the title compound was studied in detail.The single-crystal X-ray diffraction revealed that the compound crystallizes in monoclinic,space group P21/n,with a = 14.4481(7),b = 8.0089(5),c = 16.6808(9) A,α = 90.00(5),β = 100.069(5),γ = 90.00(5)°,Mr = 390.38,V = 1900.46(18) A^3,Z = 4,Dc = 1.364 g/cm^-3,μ = 0.098,F(000) = 816.0,the final R = 0.0530 and w R = 0.1141 for 2525 observed reflections(I 〉 2σ(I)),R(all data) = 0.0813,w R(all data) = 0.1335,completeness to theta of 26.020 is 99.8% and GOF = 1.085.The crystal structure contains three branched chains with its center placed at the midpoint of N.The phenyl ring(C(8)~C(13)) makes a dihedral angle of 83.5(1) ℃ with the phenyl ring(C(1)~C(6)),and 80.5(1) ℃with the nitro-substituted benzene ring(C(17)~C(22)),indicating that the three rings are not coplanar.Hydrogen bonds(C(10)–H(10)···O(3)),(C(15)–H(15B)···O(4) and C(16)–H(16B)···O(4)) together with π-π stacking interactions stabilize the structure of the molecule.The preliminary biological test shows that the title compound has good antitumor activity against A549 in vitro with the IC50 value of 3.17 μmol.
基金support from the Natural Science Foundation of Gansu Province(No.3ZS061- A25-019)the Scientific Research fund of Gansu Provincial Education Department(No.0601-25)