Solvent extraction of palladium (Ⅱ) from hydrochloric acid solution with 2-n-octyl-4-isothiazolin-3-one (OIT)/cyclohexane was studied. Effects of different parameters on extraction efficiency were evaluated. 99.9...Solvent extraction of palladium (Ⅱ) from hydrochloric acid solution with 2-n-octyl-4-isothiazolin-3-one (OIT)/cyclohexane was studied. Effects of different parameters on extraction efficiency were evaluated. 99.96 % and 98.26 % palladium (Ⅱ) could be effectively extracted with 0.018 mol·L^-1 OIT/cyclohexane of 0.1 and 4.0 mol·L^-1 HCl medium, respectively. Nonpolar solvent and low acidity could improve the extracting efficiency, and successfully strip palladium (Ⅱ) from the loaded organic phase was achieved with 0.5 mol·L^-1 (NH2)2CS solution. It was proposed that the extraction of Pd com-plexes from HCl medium proceeded through the ion-association mechanism by slope method, NMR and FF-IR spectra.展开更多
Twelve Mannich base derivatives of 1,2-benzisothiazolin-3-one were synthesized by the reaction of 1,2-benzisothiazol-3(2H)-one (BIT) with different amines and formaldehyde. All the compounds were characterized by ...Twelve Mannich base derivatives of 1,2-benzisothiazolin-3-one were synthesized by the reaction of 1,2-benzisothiazol-3(2H)-one (BIT) with different amines and formaldehyde. All the compounds were characterized by elemental analysis, IR spectroscopy, MS and 1H NMR. The crystal structure for 2,2'-methylenebis(benzo[d]isothiazol-3(2H)-one) (3) has been determined by X-ray single-crystal structure analysis. Compound 3 (C15HIoN202S2) crystallizes in the monoclinic system, space group C2/c with a = 25.052(8), b = 4.510(1), c = 11.948(4) A, β = 100.992(4)°, V= 1325.2(7) A3, Mr = 314.37, Dc = 1.576 Mg.m-3, p = 0.25 mm-1, F(000) = 648, Z = 4, R = 0.034 and wR = 0.087. The preliminary biological test indicated that the compounds (2b, 2c) showed growth inhibitory activity against the gram-positive and gram-negative bacteria.展开更多
New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<s...New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).展开更多
New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<s...New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).展开更多
Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3...Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.展开更多
The 3?Nitro?1,2,4?triazole?5?one(NTO)is a high energy density materials of keen interest for both commercial and scientific worlds owing to its reduced sensitivity,better thermal stability and high performances. It pl...The 3?Nitro?1,2,4?triazole?5?one(NTO)is a high energy density materials of keen interest for both commercial and scientific worlds owing to its reduced sensitivity,better thermal stability and high performances. It plays a significant role to replace the current energetic ingredients. In this review,we summarize various strategies involved in the synthesis of NTO as well as the existing approaches to tailor its particle morphology and sizes. The most prominent properties of NTO,such as insensitivity and performance,which are usually required to produce efficient formulations,have been concisely discussed. In addition,this overview reports on some newer forms of NTO including derivatives and co?crystals available in the literature,which can enhance the NTO features and extend its applications. The advantages and shortcomings of various NTO forms for specific and potential use are also highlighted together with the attempts made to overcome these issues. Therefore,efforts will certainly continue to improve characteristics and performances of NTO either by chemical modification or by co?crystallization in order to produce promising formulations for widespread applications in the near future.展开更多
The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4(3H)-one (C16H18N2O3, Mr = 286.32) has been prepared and determined by singlecrystal X-ray diffraction. The crystal is ...The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4(3H)-one (C16H18N2O3, Mr = 286.32) has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167(14), b = 13.113(1), c = 8.378(1) A, β = 98.992(2)^o, V = 1488.4(3) A^3, Z = 4, Dc = 1.278, F(000) = 608, μ = 0.089 mm^-1, MoKa radiation (2 = 0.71073), R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.展开更多
A new one-pot neat synthesis of some 5-aryl-2,4-dihydro-3H- 1,2,4-triazol-3-ones through cyclocondensation of ethyl carbazate with aryl nitriles catalyzed by DMAP as an efficient and basic nucleophilic catalyst is des...A new one-pot neat synthesis of some 5-aryl-2,4-dihydro-3H- 1,2,4-triazol-3-ones through cyclocondensation of ethyl carbazate with aryl nitriles catalyzed by DMAP as an efficient and basic nucleophilic catalyst is described.展开更多
The synthesis of 3-(2'-hydroxybutyl)isobenzofuran-1(3H)-onel from phthalicanhydride via the intermediate 3-(2'-oxoethyl) isobenzofuran-1(3H)-one 6 was described.
The single crystal of the title compound (C12H8N2O2, Mr = 212.20) has been obtained by oxidation of 2-aminophenol in methanol solution with irradiation of sunlight. The crystal belongs to monoclinic space group P21/c ...The single crystal of the title compound (C12H8N2O2, Mr = 212.20) has been obtained by oxidation of 2-aminophenol in methanol solution with irradiation of sunlight. The crystal belongs to monoclinic space group P21/c with cell dimensions of a = 12.925(2), b = 5.077(3), c = 14.768(3)? b = 99.38(1), V = 956.2(5)?, Z = 4, Dc = 1.474 g/cm3, = 0.103 mm-1, R = 0.054, wR = 0.074 for 785 observed reflections (I > 2s(I)). The molecule consists of three coplanar rings. Much different CC distances (1.494(4)?and 1.343(6) ? observed within the quinoidal ring show the pattern of bond fixation expected for the Kekule formula.展开更多
Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as ...Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as the catalysts for the synthesis of bisdihydropyrimidin -2(1H)-ones from aromatic dialdehydes,1,3-dicarbonyl compounds and urea at 90℃under solvent-free conditions.展开更多
The title compound 3-(2,4-dichlorophenyl)-4-dydroxy-3-(2,4-dichlorophenyl)-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-(2,4-dichlorophenyl-acetyl)-1-hydr...The title compound 3-(2,4-dichlorophenyl)-4-dydroxy-3-(2,4-dichlorophenyl)-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-(2,4-dichlorophenyl-acetyl)-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192(3), b = 10.5053(5), c = 10.5811(5)A,α = 71.681(10), β = 78.905(12), γ = 81.036(12)°, C15H14C1203, Mr = 313.18, V= 702.44(6)A3, Z = 2, De= 1.481 g/cm^3, F(000) = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ(I) and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O(1)-H(101)…O(2).展开更多
The title compound C18H16N4O3 (Mr = 336.35) 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 C18H16N4O3 (Mr = 336.35) 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 central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632(1), b = 7.816(1), c = 28.082(5) A,β = 96.18(1)°, V= 1665.48(51) A^3, Z= 4, Dc = 1.341 g/cm^3, F(000) = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C(11)-C(16) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0.03 A) with the dihedral angle between them of 9.8%.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 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
An efficient synthesis of symmetrical 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions...An efficient synthesis of symmetrical 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions at room temperature by grinding, which provides an efficient route to the synthesis of symmetrical 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one.This procedure offers several advantages including solvent-free conditions,excellent yields of products,simple work-up as well as reuse of catalysts which makes it a useful and attractive protocol for the synthesis of these compounds.展开更多
The title compound 3a-hydroxy-3-phenyl-1,2,3,3a,8a-pentahydrocyclopenta[α]- inden-8-one 2 (C18H16O2, Mr = 264.31) has been obtained by the treatment of 2-(3-iodopropyl)-2- phenylindan-1,3-dione 1 with tributylt...The title compound 3a-hydroxy-3-phenyl-1,2,3,3a,8a-pentahydrocyclopenta[α]- inden-8-one 2 (C18H16O2, Mr = 264.31) has been obtained by the treatment of 2-(3-iodopropyl)-2- phenylindan-1,3-dione 1 with tributyltin hydride in refluxing benzene, and its crystal structure was determined by single-crystal X-ray diffraction. The analysis was carried out by direct and Fourier methods and the structure was refined by full-matrix least-squares computations. The title com- pound crystallizes in monoclinic, space group P21/n with a = 9.947(3), b = 10.336(3), c = 13.239(4) ?, β = 95.565(6)o, V = 1354.7(7) ?3, Z = 4, Dc = 1.296 g/cm3, μ(MoKα) = 0.083 mm-1, F(000) = 560, the final R = 0.0749 and wR = 0.1191. X-ray analysis revealed that the bond length of O(2)– C(12) is 1.219(2) ?, slightly longer than that of the normal C=O bond (1.119 ?). The dihedral angle between planes II and III is almost 180°, while plane II is almost vertical to plane I consisting of C(1), C(3), C(4) and C(5) with the deviation of C(2) being 0.6269 ?. In addition, there exist inter- molecular hydrogen bonds between O(2) and H(1)–O(1) in the crystal structure.展开更多
A novel series of pyrido[ 1,2-e]purin-4(3H)-one derivatives containing polar substituents on 5'-position were designed and prepared as potential PDE5 inhibitors. This paper reports the synthetic routes, 1H-NMR data...A novel series of pyrido[ 1,2-e]purin-4(3H)-one derivatives containing polar substituents on 5'-position were designed and prepared as potential PDE5 inhibitors. This paper reports the synthetic routes, 1H-NMR data, and the PDE5 inhibitory activities of the target compounds. The polar piperazinyl group contained (on 5'-position) compound, 3B2, showed the highest activity among the tested derivatives but less potency than sildenafil 1.展开更多
基金financially supported by the National Natural Science Foundation of China(No.21271073)
文摘Solvent extraction of palladium (Ⅱ) from hydrochloric acid solution with 2-n-octyl-4-isothiazolin-3-one (OIT)/cyclohexane was studied. Effects of different parameters on extraction efficiency were evaluated. 99.96 % and 98.26 % palladium (Ⅱ) could be effectively extracted with 0.018 mol·L^-1 OIT/cyclohexane of 0.1 and 4.0 mol·L^-1 HCl medium, respectively. Nonpolar solvent and low acidity could improve the extracting efficiency, and successfully strip palladium (Ⅱ) from the loaded organic phase was achieved with 0.5 mol·L^-1 (NH2)2CS solution. It was proposed that the extraction of Pd com-plexes from HCl medium proceeded through the ion-association mechanism by slope method, NMR and FF-IR spectra.
基金Supported by the National Natural Science Foundation of China(No.20962007)Natural Science Foundation of Hainan Province(No.214024)
文摘Twelve Mannich base derivatives of 1,2-benzisothiazolin-3-one were synthesized by the reaction of 1,2-benzisothiazol-3(2H)-one (BIT) with different amines and formaldehyde. All the compounds were characterized by elemental analysis, IR spectroscopy, MS and 1H NMR. The crystal structure for 2,2'-methylenebis(benzo[d]isothiazol-3(2H)-one) (3) has been determined by X-ray single-crystal structure analysis. Compound 3 (C15HIoN202S2) crystallizes in the monoclinic system, space group C2/c with a = 25.052(8), b = 4.510(1), c = 11.948(4) A, β = 100.992(4)°, V= 1325.2(7) A3, Mr = 314.37, Dc = 1.576 Mg.m-3, p = 0.25 mm-1, F(000) = 648, Z = 4, R = 0.034 and wR = 0.087. The preliminary biological test indicated that the compounds (2b, 2c) showed growth inhibitory activity against the gram-positive and gram-negative bacteria.
文摘New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).
文摘New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).
基金Supported by the National Natural Science Foundation of China (No. 20962007)the Creative Talents Plan of Hainan University 211 Project
文摘Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.
文摘The 3?Nitro?1,2,4?triazole?5?one(NTO)is a high energy density materials of keen interest for both commercial and scientific worlds owing to its reduced sensitivity,better thermal stability and high performances. It plays a significant role to replace the current energetic ingredients. In this review,we summarize various strategies involved in the synthesis of NTO as well as the existing approaches to tailor its particle morphology and sizes. The most prominent properties of NTO,such as insensitivity and performance,which are usually required to produce efficient formulations,have been concisely discussed. In addition,this overview reports on some newer forms of NTO including derivatives and co?crystals available in the literature,which can enhance the NTO features and extend its applications. The advantages and shortcomings of various NTO forms for specific and potential use are also highlighted together with the attempts made to overcome these issues. Therefore,efforts will certainly continue to improve characteristics and performances of NTO either by chemical modification or by co?crystallization in order to produce promising formulations for widespread applications in the near future.
基金This work was supported by the Natural Science Foundation of Hubei Province (2006ABB016)National Natural Science Foundation of China (20672041) Key Project of Science and Technology of Ministry of Education of China (107082, 106116)
文摘The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4(3H)-one (C16H18N2O3, Mr = 286.32) has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167(14), b = 13.113(1), c = 8.378(1) A, β = 98.992(2)^o, V = 1488.4(3) A^3, Z = 4, Dc = 1.278, F(000) = 608, μ = 0.089 mm^-1, MoKa radiation (2 = 0.71073), R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.
文摘A new one-pot neat synthesis of some 5-aryl-2,4-dihydro-3H- 1,2,4-triazol-3-ones through cyclocondensation of ethyl carbazate with aryl nitriles catalyzed by DMAP as an efficient and basic nucleophilic catalyst is described.
文摘The synthesis of 3-(2'-hydroxybutyl)isobenzofuran-1(3H)-onel from phthalicanhydride via the intermediate 3-(2'-oxoethyl) isobenzofuran-1(3H)-one 6 was described.
基金The work was supported by the National Natural Science Foundation of China (29973036)
文摘The single crystal of the title compound (C12H8N2O2, Mr = 212.20) has been obtained by oxidation of 2-aminophenol in methanol solution with irradiation of sunlight. The crystal belongs to monoclinic space group P21/c with cell dimensions of a = 12.925(2), b = 5.077(3), c = 14.768(3)? b = 99.38(1), V = 956.2(5)?, Z = 4, Dc = 1.474 g/cm3, = 0.103 mm-1, R = 0.054, wR = 0.074 for 785 observed reflections (I > 2s(I)). The molecule consists of three coplanar rings. Much different CC distances (1.494(4)?and 1.343(6) ? observed within the quinoidal ring show the pattern of bond fixation expected for the Kekule formula.
文摘Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as the catalysts for the synthesis of bisdihydropyrimidin -2(1H)-ones from aromatic dialdehydes,1,3-dicarbonyl compounds and urea at 90℃under solvent-free conditions.
基金Supported by the Natural Science Foundation of Zhejiang Province (2008C21029)
文摘The title compound 3-(2,4-dichlorophenyl)-4-dydroxy-3-(2,4-dichlorophenyl)-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-(2,4-dichlorophenyl-acetyl)-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192(3), b = 10.5053(5), c = 10.5811(5)A,α = 71.681(10), β = 78.905(12), γ = 81.036(12)°, C15H14C1203, Mr = 313.18, V= 702.44(6)A3, Z = 2, De= 1.481 g/cm^3, F(000) = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ(I) and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O(1)-H(101)…O(2).
文摘The title compound C18H16N4O3 (Mr = 336.35) 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 central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632(1), b = 7.816(1), c = 28.082(5) A,β = 96.18(1)°, V= 1665.48(51) A^3, Z= 4, Dc = 1.341 g/cm^3, F(000) = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C(11)-C(16) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0.03 A) with the dihedral angle between them of 9.8%.
基金We gratefully acknowledge financial support of this work by the National Key Project for Basic Research(2003CB114400,2003CB114406)the National Natural Science Foundation of China(Project No.20102001).
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 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 research foundation of Hebei University of Science and Technology
文摘An efficient synthesis of symmetrical 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions at room temperature by grinding, which provides an efficient route to the synthesis of symmetrical 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one.This procedure offers several advantages including solvent-free conditions,excellent yields of products,simple work-up as well as reuse of catalysts which makes it a useful and attractive protocol for the synthesis of these compounds.
基金The project was supported by the Key Laboratory of Organic Synthesis of Jiangsu Province (JSK016)
文摘The title compound 3a-hydroxy-3-phenyl-1,2,3,3a,8a-pentahydrocyclopenta[α]- inden-8-one 2 (C18H16O2, Mr = 264.31) has been obtained by the treatment of 2-(3-iodopropyl)-2- phenylindan-1,3-dione 1 with tributyltin hydride in refluxing benzene, and its crystal structure was determined by single-crystal X-ray diffraction. The analysis was carried out by direct and Fourier methods and the structure was refined by full-matrix least-squares computations. The title com- pound crystallizes in monoclinic, space group P21/n with a = 9.947(3), b = 10.336(3), c = 13.239(4) ?, β = 95.565(6)o, V = 1354.7(7) ?3, Z = 4, Dc = 1.296 g/cm3, μ(MoKα) = 0.083 mm-1, F(000) = 560, the final R = 0.0749 and wR = 0.1191. X-ray analysis revealed that the bond length of O(2)– C(12) is 1.219(2) ?, slightly longer than that of the normal C=O bond (1.119 ?). The dihedral angle between planes II and III is almost 180°, while plane II is almost vertical to plane I consisting of C(1), C(3), C(4) and C(5) with the deviation of C(2) being 0.6269 ?. In addition, there exist inter- molecular hydrogen bonds between O(2) and H(1)–O(1) in the crystal structure.
文摘A novel series of pyrido[ 1,2-e]purin-4(3H)-one derivatives containing polar substituents on 5'-position were designed and prepared as potential PDE5 inhibitors. This paper reports the synthetic routes, 1H-NMR data, and the PDE5 inhibitory activities of the target compounds. The polar piperazinyl group contained (on 5'-position) compound, 3B2, showed the highest activity among the tested derivatives but less potency than sildenafil 1.