The title compound C18H18N4OS has been synthesized by the reaction of 3-（2-hydroxy- benzyl）-4-amino-（1H）-1,2,4-triazole-5-thione with 4-isopropylbenzaldehyde in ethanol and characterized by IR, ^1H NMR spectra and...The title compound C18H18N4OS has been synthesized by the reaction of 3-（2-hydroxy- benzyl）-4-amino-（1H）-1,2,4-triazole-5-thione with 4-isopropylbenzaldehyde in ethanol and characterized by IR, ^1H NMR spectra and elemental analysis. Its structure was determined by X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 11.605（2）, b = 7.401（1）, c = 20.339（2） A, β= 103.05（2）°, V= 1701.8（4） A^3, Z = 4, Mr = 338.42,μ = 0.202 mm^-1, Dc = 1.321 g/cm^3 and F（000） = 712. The structure was solved by direct methods and refined to R = 0.0428 and wR = 0.1069. Due to the intramolecular O-H…N hydrogen bond and π-π stacking interactions between the benzene （C（1）～C（6）） and triazole rings, the two planes are essentially coplanar. Their biological activities have been measured, showing this type of compound has certain antibacterial activity for Staphylococous aureus and Bacillus subtilis. Based on the quantum chemistry calculation at the RHF/6-31G level, the frontier orbitals and electrostatic potential of the title compound were also discussed.展开更多
The crystal structure of a (3-phenylureido)-a (2, 4-dichlorophenyl)methyl phenylphosphinic acid, C20H17Cl2N2O3P, Mr= 435. 25,which was obtained bydesulphurisation of cis-3, 4-dipheny1-5- (2, 4-dichlorophenyl ) -1, 3, ...The crystal structure of a (3-phenylureido)-a (2, 4-dichlorophenyl)methyl phenylphosphinic acid, C20H17Cl2N2O3P, Mr= 435. 25,which was obtained bydesulphurisation of cis-3, 4-dipheny1-5- (2, 4-dichlorophenyl ) -1, 3, 4-diazaphospholidin2-thione-4-oxide utilizing Ag+ -H2O system in a yield of 89%, is reported. It crystallizes in orthorhombic space group Pca21 with a= 11. 286(2), b= 20. 601 (4) f c=8. 695(2)A, V= 2021 (1) A3, Z= 4, D.= 1. 430 g/cm3, p=4. 21 cm-1, F(000) =896.The final R factor is 0. 040 and Rw is 0. 045 for 946 unique observed reflections[I>3a(I)]. The result of X-ray analysis indicates that the molecules in the crystal are linkedtogether by the O(3 ) ...H (2d) - N (2d ) intermolecular hydrogen-bondings.展开更多
A self-intermolecular cyclocondensation reaction of 3,4-dihydropyrimidine-2-thione（DHPM） to give a novel tricyclic structure containing DHPM core in the presence of diethyl azodicarboxylate（DEAD） and triphenylphos...A self-intermolecular cyclocondensation reaction of 3,4-dihydropyrimidine-2-thione（DHPM） to give a novel tricyclic structure containing DHPM core in the presence of diethyl azodicarboxylate（DEAD） and triphenylphosphine（TPP） at room temperature is reported.展开更多
An efficient method for the synthesis of novel benzo[b]pyrido[3＇,2＇：4,5]thieno[2,3-e][l,6]naphthyridine-8-one derivatives has been developed using a Pictet-Spengler reaction between 4-（3-aminothieno[2,3-b]pyridin-...An efficient method for the synthesis of novel benzo[b]pyrido[3＇,2＇：4,5]thieno[2,3-e][l,6]naphthyridine-8-one derivatives has been developed using a Pictet-Spengler reaction between 4-（3-aminothieno[2,3-b]pyridin-2-yl）quinoline-2-ones,which could be obtained from the alkylation of4-bromomethylquinoline-2-ones with 3-cyanopyridine-2-thione followed by a Thorpe-Ziegler isomerization,and aromatic aldehydes under p-TsOH as catalysis in good yields.展开更多
An efficient method for the synthesis of novel pyrido[3＇＇,2＇＇：4＇,5＇]thieno[3＇,2＇：2,3]pyrido [4,5：d][1,3]thiazolo[3,2-a]pyrimidine-4-one derivatives（5） has been developed using a Pictet–Spengler reaction ...An efficient method for the synthesis of novel pyrido[3＇＇,2＇＇：4＇,5＇]thieno[3＇,2＇：2,3]pyrido [4,5：d][1,3]thiazolo[3,2-a]pyrimidine-4-one derivatives（5） has been developed using a Pictet–Spengler reaction between 2-（3-aminothieno[2,3-b]pyridin-2-yl）thiazolo[3,2-a] pyrimidin-5-one（3）, which could be obtained from the condensation of 7-（chloromethyl）-5H-thiazolo[3,2-a]pyrimidin-5-one（1） with3-cyanopyridine-2-thione（2） via Thorpe–Ziegler isomerization, and aromatic aldehydes under NH2SO3 H as catalysis in good yields.展开更多
基金This work was supported by the Natural Science Foundation of Zhejiang Province (No. M203115) and Scientific Research Fund of Zhejiang Provincial Education Department (No. 20050057)
文摘The title compound C18H18N4OS has been synthesized by the reaction of 3-（2-hydroxy- benzyl）-4-amino-（1H）-1,2,4-triazole-5-thione with 4-isopropylbenzaldehyde in ethanol and characterized by IR, ^1H NMR spectra and elemental analysis. Its structure was determined by X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 11.605（2）, b = 7.401（1）, c = 20.339（2） A, β= 103.05（2）°, V= 1701.8（4） A^3, Z = 4, Mr = 338.42,μ = 0.202 mm^-1, Dc = 1.321 g/cm^3 and F（000） = 712. The structure was solved by direct methods and refined to R = 0.0428 and wR = 0.1069. Due to the intramolecular O-H…N hydrogen bond and π-π stacking interactions between the benzene （C（1）～C（6）） and triazole rings, the two planes are essentially coplanar. Their biological activities have been measured, showing this type of compound has certain antibacterial activity for Staphylococous aureus and Bacillus subtilis. Based on the quantum chemistry calculation at the RHF/6-31G level, the frontier orbitals and electrostatic potential of the title compound were also discussed.
文摘The crystal structure of a (3-phenylureido)-a (2, 4-dichlorophenyl)methyl phenylphosphinic acid, C20H17Cl2N2O3P, Mr= 435. 25,which was obtained bydesulphurisation of cis-3, 4-dipheny1-5- (2, 4-dichlorophenyl ) -1, 3, 4-diazaphospholidin2-thione-4-oxide utilizing Ag+ -H2O system in a yield of 89%, is reported. It crystallizes in orthorhombic space group Pca21 with a= 11. 286(2), b= 20. 601 (4) f c=8. 695(2)A, V= 2021 (1) A3, Z= 4, D.= 1. 430 g/cm3, p=4. 21 cm-1, F(000) =896.The final R factor is 0. 040 and Rw is 0. 045 for 946 unique observed reflections[I>3a(I)]. The result of X-ray analysis indicates that the molecules in the crystal are linkedtogether by the O(3 ) ...H (2d) - N (2d ) intermolecular hydrogen-bondings.
基金financial support from the National Nature Science Foundation of China(No.20902073)the Natural Science Foundation of Gansu Province(No.096RJZA116)Scientific and Technological Innovation Engineering program of Northwest Normal University(nwnu-kjcxgc-03-64)
文摘A self-intermolecular cyclocondensation reaction of 3,4-dihydropyrimidine-2-thione（DHPM） to give a novel tricyclic structure containing DHPM core in the presence of diethyl azodicarboxylate（DEAD） and triphenylphosphine（TPP） at room temperature is reported.
文摘An efficient method for the synthesis of novel benzo[b]pyrido[3＇,2＇：4,5]thieno[2,3-e][l,6]naphthyridine-8-one derivatives has been developed using a Pictet-Spengler reaction between 4-（3-aminothieno[2,3-b]pyridin-2-yl）quinoline-2-ones,which could be obtained from the alkylation of4-bromomethylquinoline-2-ones with 3-cyanopyridine-2-thione followed by a Thorpe-Ziegler isomerization,and aromatic aldehydes under p-TsOH as catalysis in good yields.
文摘An efficient method for the synthesis of novel pyrido[3＇＇,2＇＇：4＇,5＇]thieno[3＇,2＇：2,3]pyrido [4,5：d][1,3]thiazolo[3,2-a]pyrimidine-4-one derivatives（5） has been developed using a Pictet–Spengler reaction between 2-（3-aminothieno[2,3-b]pyridin-2-yl）thiazolo[3,2-a] pyrimidin-5-one（3）, which could be obtained from the condensation of 7-（chloromethyl）-5H-thiazolo[3,2-a]pyrimidin-5-one（1） with3-cyanopyridine-2-thione（2） via Thorpe–Ziegler isomerization, and aromatic aldehydes under NH2SO3 H as catalysis in good yields.
