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
4-Hydroxybenzoate (4HBA) is a naturally occurring aromatic compound, as a key intermediate metabolite not only for natural products but also for arti- ficial products. There are four metabolic pathways for 4HBA: pr...4-Hydroxybenzoate (4HBA) is a naturally occurring aromatic compound, as a key intermediate metabolite not only for natural products but also for arti- ficial products. There are four metabolic pathways for 4HBA: protocatechuate cleavage pathway; catechol cleavage pathway; anaerobic degradation pathway in anaerobes ; and gentisate cleavage pathway. The last pathway including a NIH shift reaction remains to be elucidated. In this review we emphasized on the NIH shift reaction involved in the 4HBA degrdation. The key enzymes of each 4HBA metabolic pathway also were introduced. Finnaly, we described the thermophilic Bacillus sp. B1 strain which was capable of degrading varous aromatic compounds including gHBA, and presented a direction for the research of NIH shift reaction.展开更多
The title compound (ethyl5-(4-(2-phenylacetamido)phenyl)-lH-pyrazole-3-carboxylate, C20H19N3O3) was synthesized by the reaction of Claisen condensation, cyclization, reduction and acylation. The structure was ch...The title compound (ethyl5-(4-(2-phenylacetamido)phenyl)-lH-pyrazole-3-carboxylate, C20H19N3O3) was synthesized by the reaction of Claisen condensation, cyclization, reduction and acylation. The structure was characterized by X-ray diffraction, MS, NMR and IR. It belongs to the monoclinic system, space group C2/c with a = 22.723(9), b = 9.324(4), c = 18.890(8) A, β = 114.259(6)°, V = 3649(3) A^3, Dc = 1.272 Mg·m^3, Z = 8, Mr = 349.38, p = 0.087 mm^-1, F(000) = 1472, the final R = 0.0615 and wR = 0.1643. The biological test shows that the title compound has a moderate acrosin inhibition activity.展开更多
The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined...The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215(9), b = 8.5311(4), c = 21.6886(9) A^°, β = 91.607(1)°, V = 3814.0(3)A^°^3, Z = 8, Dc = 1.400 g/cm^3, F(000) = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.展开更多
A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravim...A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravimetric analysis,fluorescence spectrum,and singlecrystal X-ray diffraction.Yellow crystal crystallizes in the orthorhombic system,space group Pbca with a = 16.220(5),b = 14.980(5),c = 20.521(5) ?,V = 4986(3) ?~3,C(24)H(26)CdN4O7,Mr = 594.89,Dc = 1.585 g/cm^3,μ(Mo Kα) = 0.927 mm^(-1),F(000) = 2416,Z = 8,the final R = 0.0242 and w R = 0.0589 for 4076 observed reflections(I 〉 2s(I)).In 1,the Cd(Ⅱ) ion takes a six-coordination mode,and bib ligand bridges adjacent Cd(Ⅱ) ions to generate 1D zigzag chains; these neighboring chains are connected by O–H···O hydrogen bonding interactions,producing a 2D folded layered structure.Furthermore,by O–H···O hydrogen bonding between layers and layers,a 3D supramolecular architecture is formed.In addition,we analyzed Natural Bond Orbital(NBO) in using the PBE0/LANL2 DZ method built in Gaussian 03 Program.The calculation results indicated obvious covalent interaction between the coordinated atoms and Cd(Ⅱ) ion.展开更多
The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H1...The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H15N2O3)3(H2O)]DMFH2O. The coordi- nation sphere about each copper ion in the complex consists of two oxygen atoms from hydroxylpyridinone moiety of one ligand and one oxygen and one nitrogen atoms from salicyladehyde Schiff-base moiety of another ligand arranged in a slightly distorted square planar geometry. Among the three copper ions, one (Cu(2)) is coordinated by the other oxygen atom of water molecule on the fifth coordinate position to form a distorted square pyramid geometry. The crystal is of monoclinic, space group P21/c with a = 12.9202(5), b = 27.197(1), c = 17.0116(7) ? b = 100.588(1), V = 5875.9(4) 3, Z = 4, C63H57N7O12Cu3, Mr = 1294.78, Dc = 1.464 g/cm3, m = 1.146 mm-1, F(000) = 2668, R = 0.0784 and wR = 0.1546 for 6926 observed reflections with I > 2s(I). The differences of coordinate bond lengths are observed between anhydrous and hydrous units: in the former unit, the average bond lengths are 1.978 ?for CuN (azomethine), 1.883 ?for CuO (phenolic) in Schiff-base moiety, 1.959 ?for CuO (keto), and 1.919 ?for CuO (hydroxy) in hydroxypyridinone moiety; while those in the latter are longer with the following corresponding values: 1.985(5), 1.908(5), 1.993(5) and 1.919(4) ? respectively. The Cu(2)O (water) bond length is 2.375(6) ?展开更多
One of the phenolic acids is 4-hydroxybenzoic acid(HBA)which takes the form of a white crystalline solid with a molecular formula of C 7H 6O 3,a melting point of 214.5℃and a molecular weight of 138.12 g·mol^(-1)...One of the phenolic acids is 4-hydroxybenzoic acid(HBA)which takes the form of a white crystalline solid with a molecular formula of C 7H 6O 3,a melting point of 214.5℃and a molecular weight of 138.12 g·mol^(-1).It soluble in polar organic solvents like acetone and alcohols,and slightly soluble in chloroform and water.The reactions between the metal ions and the HBA were carried out under specific conditions like(molar reaction was 2∶2(ligand to metal),reaction temperature was 60℃,media was neutral(pH 7),and solvent was H 2O∶MeOH(1∶1).Under these conditions,the HBA was deprotonated to form(HOC_(6)H_(4)CO^(2);L^(-)).The ligand L-was coordinated to the metal ions forming the metal complexation.The reaction of 4-hydroxybenzoic acid(HOC 6H 4CO 2H;HL)with the Ni(Ⅱ),Mn(Ⅱ)and Cu(Ⅱ)ions afford metal-complexes with gross formula of[Ni_(2)L_(2)(NO_(3))_(2)(H_(2)O)_(4)],[Mn_(2)L_(2)(NO_(3))_(2)(H_(2)O)_(4)]and[Cu_(2)L_(2)(NO_(3))_(2)(H_(2)O)_(4)],respectively.These complexes were characterized by elemental analysis(CHN),magnetic susceptibility,UV-Vis spectra,infrared(IR),and X-ray powder diffraction(XRD)techniques.The complexes of HBA are insoluble in common solvents and hence molar conductance could not be measured,but this very insolubility indicates that the complexes are neutral.Data has demonstrated that the ligand(L^(-))was coordinated to the metal ion by bidentate bridging carboxylate group(COO^(-)),with an octahedral geometry.Thus,HBA is expected to act as bidentate uninegative ions and the coordination number of the metal ions is six.XRD results showed that the complexes possess uniform and organized microstructures in the nanometer range with a main diameter in the range of 11~28 nm.展开更多
The extraction and stripping of scandium from its sulfate solutions by isopropyl phosphonic acid mono (1-hexyl-4-ethyl) octyl ester (PT-2, HL) diluted with n-hexane are reported. A high efficiency of separation betwee...The extraction and stripping of scandium from its sulfate solutions by isopropyl phosphonic acid mono (1-hexyl-4-ethyl) octyl ester (PT-2, HL) diluted with n-hexane are reported. A high efficiency of separation between scandium, iron and lutetium can be achieved by controlling aqueous acidity. Different mechanisms of Sc3+ with PT-2 in various acid range have been proposed.At lower aqueous acidity, it is a cation exchange reaction, while at higher acidity. a solvation reaction was ascertained. Its IR and NMR spectra have been discussed. The effect of temperature on extraction of Sc3+ was observed and thermodynamic functions were calculated.展开更多
The title compound ethyl 2-(6-(1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2(3H)- yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate 3 was synthesized by the reaction of ethyl 2-(6-amino-7-fluoro-3-ox...The title compound ethyl 2-(6-(1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2(3H)- yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate 3 was synthesized by the reaction of ethyl 2-(6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate with 4,5,6,7- tetraydrophthalic anhydride, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2 1/n with a = 9.3469(2), b = 16.7715(5), c = 13.7153(4) A, β= 104.9680(10)°, μ = 0.107 mm^-1, Mr = 430.42, V= 2077.08(10) ,A3, Z= 4, Dc = 1.376 g/cm3, F(000) = 904, T= 296(2) K, R = 0.0508 and wR = 0.1478.展开更多
4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single ...4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data: C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309(3), b = 0.67682(6), c = 1.74237(19) nm, β = 114.744(3)°, V= 2.7106(5) nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F(000) = 1200, Z= 8, R= 0.0514 and wR= 0.1529.展开更多
Ethyl ester of 5,7-dimethyl coumarin-4-acetic acid has been synthesized from 3,5-Xylenol in a two step sequence of reaction involving Pechmann cyclisation and acid catalyzed esterification. The title compound 2 crysta...Ethyl ester of 5,7-dimethyl coumarin-4-acetic acid has been synthesized from 3,5-Xylenol in a two step sequence of reaction involving Pechmann cyclisation and acid catalyzed esterification. The title compound 2 crystallizes in Monoclinic form, space group P 1 21/c 1, with a = 8.6248(4) ?, b = 18.9103(8) , c = 8.4204(4)?, β = 101.241(2)?, V = 1347.00(11) ?, D cal = 1.283 Mg/cm3, Z = 4. The molecule is stabilized by intermolecular C-H … O bonds.展开更多
The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffract...The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1, with a = 8.140(3), b = 11.966(4), c = 13.771(5)Aα= 67.366(4), β= 85.165(5), γ= 75.806(4)°, V = 1200.1(7) A3, Z = 2, C26H3008, Mr = 470.50, Dc = 1.302 g/cm^3, F(000) = 500,λ(MoKa) = 0.71073 A, μ= 0.096 mm^-1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections (I 〉 2σ(I)). As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.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Supported by the National Natural Science Foundation of China(31400099)Jiangsu Science and Technology Agency Project(BK20141148 and BK20140235)Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions(PAPD)
文摘4-Hydroxybenzoate (4HBA) is a naturally occurring aromatic compound, as a key intermediate metabolite not only for natural products but also for arti- ficial products. There are four metabolic pathways for 4HBA: protocatechuate cleavage pathway; catechol cleavage pathway; anaerobic degradation pathway in anaerobes ; and gentisate cleavage pathway. The last pathway including a NIH shift reaction remains to be elucidated. In this review we emphasized on the NIH shift reaction involved in the 4HBA degrdation. The key enzymes of each 4HBA metabolic pathway also were introduced. Finnaly, we described the thermophilic Bacillus sp. B1 strain which was capable of degrading varous aromatic compounds including gHBA, and presented a direction for the research of NIH shift reaction.
基金supported by the Science and technology support program of Jiangsu Province (2010, BE2010682)
文摘The title compound (ethyl5-(4-(2-phenylacetamido)phenyl)-lH-pyrazole-3-carboxylate, C20H19N3O3) was synthesized by the reaction of Claisen condensation, cyclization, reduction and acylation. The structure was characterized by X-ray diffraction, MS, NMR and IR. It belongs to the monoclinic system, space group C2/c with a = 22.723(9), b = 9.324(4), c = 18.890(8) A, β = 114.259(6)°, V = 3649(3) A^3, Dc = 1.272 Mg·m^3, Z = 8, Mr = 349.38, p = 0.087 mm^-1, F(000) = 1472, the final R = 0.0615 and wR = 0.1643. The biological test shows that the title compound has a moderate acrosin inhibition activity.
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. 2006QDJ16)
文摘The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215(9), b = 8.5311(4), c = 21.6886(9) A^°, β = 91.607(1)°, V = 3814.0(3)A^°^3, Z = 8, Dc = 1.400 g/cm^3, F(000) = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.
基金supported by the Science and Technology Development Project of Jilin Provincial Science&Technology Department(201205080)the Science and Technology Research Projects of the Education Office of Jilin Province(No.2013.384)
文摘A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravimetric analysis,fluorescence spectrum,and singlecrystal X-ray diffraction.Yellow crystal crystallizes in the orthorhombic system,space group Pbca with a = 16.220(5),b = 14.980(5),c = 20.521(5) ?,V = 4986(3) ?~3,C(24)H(26)CdN4O7,Mr = 594.89,Dc = 1.585 g/cm^3,μ(Mo Kα) = 0.927 mm^(-1),F(000) = 2416,Z = 8,the final R = 0.0242 and w R = 0.0589 for 4076 observed reflections(I 〉 2s(I)).In 1,the Cd(Ⅱ) ion takes a six-coordination mode,and bib ligand bridges adjacent Cd(Ⅱ) ions to generate 1D zigzag chains; these neighboring chains are connected by O–H···O hydrogen bonding interactions,producing a 2D folded layered structure.Furthermore,by O–H···O hydrogen bonding between layers and layers,a 3D supramolecular architecture is formed.In addition,we analyzed Natural Bond Orbital(NBO) in using the PBE0/LANL2 DZ method built in Gaussian 03 Program.The calculation results indicated obvious covalent interaction between the coordinated atoms and Cd(Ⅱ) ion.
基金This work was supported by the foundation of Natural Science Research of Jiangsu Education Department (02KJB150007)
文摘The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H15N2O3)3(H2O)]DMFH2O. The coordi- nation sphere about each copper ion in the complex consists of two oxygen atoms from hydroxylpyridinone moiety of one ligand and one oxygen and one nitrogen atoms from salicyladehyde Schiff-base moiety of another ligand arranged in a slightly distorted square planar geometry. Among the three copper ions, one (Cu(2)) is coordinated by the other oxygen atom of water molecule on the fifth coordinate position to form a distorted square pyramid geometry. The crystal is of monoclinic, space group P21/c with a = 12.9202(5), b = 27.197(1), c = 17.0116(7) ? b = 100.588(1), V = 5875.9(4) 3, Z = 4, C63H57N7O12Cu3, Mr = 1294.78, Dc = 1.464 g/cm3, m = 1.146 mm-1, F(000) = 2668, R = 0.0784 and wR = 0.1546 for 6926 observed reflections with I > 2s(I). The differences of coordinate bond lengths are observed between anhydrous and hydrous units: in the former unit, the average bond lengths are 1.978 ?for CuN (azomethine), 1.883 ?for CuO (phenolic) in Schiff-base moiety, 1.959 ?for CuO (keto), and 1.919 ?for CuO (hydroxy) in hydroxypyridinone moiety; while those in the latter are longer with the following corresponding values: 1.985(5), 1.908(5), 1.993(5) and 1.919(4) ? respectively. The Cu(2)O (water) bond length is 2.375(6) ?
基金the deanship of scientific Research at Princess Nourah bint Abdulrahman University through the Fast-track Research Funding program。
文摘One of the phenolic acids is 4-hydroxybenzoic acid(HBA)which takes the form of a white crystalline solid with a molecular formula of C 7H 6O 3,a melting point of 214.5℃and a molecular weight of 138.12 g·mol^(-1).It soluble in polar organic solvents like acetone and alcohols,and slightly soluble in chloroform and water.The reactions between the metal ions and the HBA were carried out under specific conditions like(molar reaction was 2∶2(ligand to metal),reaction temperature was 60℃,media was neutral(pH 7),and solvent was H 2O∶MeOH(1∶1).Under these conditions,the HBA was deprotonated to form(HOC_(6)H_(4)CO^(2);L^(-)).The ligand L-was coordinated to the metal ions forming the metal complexation.The reaction of 4-hydroxybenzoic acid(HOC 6H 4CO 2H;HL)with the Ni(Ⅱ),Mn(Ⅱ)and Cu(Ⅱ)ions afford metal-complexes with gross formula of[Ni_(2)L_(2)(NO_(3))_(2)(H_(2)O)_(4)],[Mn_(2)L_(2)(NO_(3))_(2)(H_(2)O)_(4)]and[Cu_(2)L_(2)(NO_(3))_(2)(H_(2)O)_(4)],respectively.These complexes were characterized by elemental analysis(CHN),magnetic susceptibility,UV-Vis spectra,infrared(IR),and X-ray powder diffraction(XRD)techniques.The complexes of HBA are insoluble in common solvents and hence molar conductance could not be measured,but this very insolubility indicates that the complexes are neutral.Data has demonstrated that the ligand(L^(-))was coordinated to the metal ion by bidentate bridging carboxylate group(COO^(-)),with an octahedral geometry.Thus,HBA is expected to act as bidentate uninegative ions and the coordination number of the metal ions is six.XRD results showed that the complexes possess uniform and organized microstructures in the nanometer range with a main diameter in the range of 11~28 nm.
文摘The extraction and stripping of scandium from its sulfate solutions by isopropyl phosphonic acid mono (1-hexyl-4-ethyl) octyl ester (PT-2, HL) diluted with n-hexane are reported. A high efficiency of separation between scandium, iron and lutetium can be achieved by controlling aqueous acidity. Different mechanisms of Sc3+ with PT-2 in various acid range have been proposed.At lower aqueous acidity, it is a cation exchange reaction, while at higher acidity. a solvation reaction was ascertained. Its IR and NMR spectra have been discussed. The effect of temperature on extraction of Sc3+ was observed and thermodynamic functions were calculated.
基金Supported by the National Natural Science Foundation of China (20872033, 20575019)Natural Science Foundation of Hunan Province (07JJ1003)+1 种基金Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China) (KLCBTCMR2008-14)Scientific Research Fund of Science and Technology Department of Hunan Province (No. 2006GK3067)
文摘The title compound ethyl 2-(6-(1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2(3H)- yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate 3 was synthesized by the reaction of ethyl 2-(6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate with 4,5,6,7- tetraydrophthalic anhydride, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2 1/n with a = 9.3469(2), b = 16.7715(5), c = 13.7153(4) A, β= 104.9680(10)°, μ = 0.107 mm^-1, Mr = 430.42, V= 2077.08(10) ,A3, Z= 4, Dc = 1.376 g/cm3, F(000) = 904, T= 296(2) K, R = 0.0508 and wR = 0.1478.
基金supported by the National Natural Science Foundation of China (20571060)Natural Science Foundation of Shaanxi Province (2007B08)Education Committee of Shaanxi Province (05JK294)
文摘4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data: C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309(3), b = 0.67682(6), c = 1.74237(19) nm, β = 114.744(3)°, V= 2.7106(5) nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F(000) = 1200, Z= 8, R= 0.0514 and wR= 0.1529.
文摘Ethyl ester of 5,7-dimethyl coumarin-4-acetic acid has been synthesized from 3,5-Xylenol in a two step sequence of reaction involving Pechmann cyclisation and acid catalyzed esterification. The title compound 2 crystallizes in Monoclinic form, space group P 1 21/c 1, with a = 8.6248(4) ?, b = 18.9103(8) , c = 8.4204(4)?, β = 101.241(2)?, V = 1347.00(11) ?, D cal = 1.283 Mg/cm3, Z = 4. The molecule is stabilized by intermolecular C-H … O bonds.
基金supported by the National Natural Science Foundation of China (No. 30572238)
文摘The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1, with a = 8.140(3), b = 11.966(4), c = 13.771(5)Aα= 67.366(4), β= 85.165(5), γ= 75.806(4)°, V = 1200.1(7) A3, Z = 2, C26H3008, Mr = 470.50, Dc = 1.302 g/cm^3, F(000) = 500,λ(MoKa) = 0.71073 A, μ= 0.096 mm^-1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections (I 〉 2σ(I)). As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.