The title compound 2-amino-5,6-dihydro-4-(3,4-dimethoxyphenyl)-4H-benzo[h]- chromene-3-carbonitrile (C22H20N2O3, Mr = 360.40) was obtained by the reaction of 2-(3,4-dimeth- oxybenzylidene)-1-tetralone and malono...The title compound 2-amino-5,6-dihydro-4-(3,4-dimethoxyphenyl)-4H-benzo[h]- chromene-3-carbonitrile (C22H20N2O3, Mr = 360.40) was obtained by the reaction of 2-(3,4-dimeth- oxybenzylidene)-1-tetralone and malononitrile in DMF in the presence of KF-montmorillonite. Its structure was confirmed by IR and ^1H NMR spectra. The crystal is of monoclinic, space group C2/c with a = 24.101(6), b = 9.146(2), c = 17.238(3) ,A, β= 95.92(2)°, Z = 8, V= 3779.4(14) ,A^3, Dc = 1.267 g/cm^3, μ(MoKa) = 0.085 mm^-1, F(000) = 1520, R = 0.0409 and wR = 0.0981 for 2043 observed reflections (I 〉 2σ(I)).展开更多
The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst...The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst under microwave irradiation. Its structure was charac- terized by X-ray single-crystal diffraction techniques with the following data: triclinic, space group P1, a = 5.4513(4), b = 7.619(1), c = 16.118(4) ?, α = 80.42(1), β = 83.43(1), γ = 79.29(1)°, V = 646.19(19) ?3, Mr = 280.70, μ(MoKα) = 0.301 mm-1, Z = 2 and Dc = 1.443 g/cm3. In the molecule the pyrimidine ring is of boat conformation.展开更多
The title compound C35H30Br2O3 (C32H24Br2O2·CH3COCH3) has been synthesized by the dimerization of 2-(4'-bromobenzal)-1-indenone induced by low-valent titanium reagent, and characterized by elemental analysis...The title compound C35H30Br2O3 (C32H24Br2O2·CH3COCH3) has been synthesized by the dimerization of 2-(4'-bromobenzal)-1-indenone induced by low-valent titanium reagent, and characterized by elemental analysis, IR,^1H NMR and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.273(7), b = 11.036(7), c = 13.944(9) ,A°, a = 73.972(9), β =76.577(10),γ= 88.871(10)°, V = 1476.3(17)A°^3, Mr = 658.41, Z = 2, Dr = 1.481 g/cm^3, μ(MoKa) = 2.780 mm^-1, F(000) = 668, the final R = 0.0452 and wR = 0.0975. X-ray analysis reveals that the two cyclopentane rings spiro-fused each other adopt envelope conformations, while the other cyclopentane ring (C(1)--C(2)-C(7)-C(9)) is coplanar. In addition, there is a classical intermolecular hydrogen bond O(1)-H(1)...O(2) connecting the adjacent molecules into dimers.展开更多
The title compound 1-(4-chlorophenyl)-2-cyano-3-amino-3a-hydroxy-3a,3b,6,7- tetrahydro-benzo[4,5]indene 2, has been synthesized by the reductive cyclization of 2-cyano-3- (4-chlorophenyl)-3-(1-tetralon-2-yl) pro...The title compound 1-(4-chlorophenyl)-2-cyano-3-amino-3a-hydroxy-3a,3b,6,7- tetrahydro-benzo[4,5]indene 2, has been synthesized by the reductive cyclization of 2-cyano-3- (4-chlorophenyl)-3-(1-tetralon-2-yl) propionitrile 1 induced by low-valent titanium reagent and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/c with a = 28.244(7), b = 14.401(3), c = 21.245(3)A,β= 115.71(2)°, V = 7786(3)A^3, Mr= 696.13, Dc = 1.188 g/cm^3, Z = 8,μ(MoKα) = 0.208 mm^-1, F(000) = 2916, R = 0.0783 and wR = 0.2350. X-ray analysis reveals that the five-membered ring (C(7)~C(l l)) adopts an envelop conformation, while the six-membered ring (C(10)~C(14), C(19)) has a half-chair conformation. Meanwhile, intermolecular H-bond interactions result in the formation of polymer.展开更多
A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation. This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3 c...A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation. This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3 carbonyl compound and urea. The structure of 4o was determined by single crystal X ray diffraction analysis.展开更多
N-Hydroxylacridinedione derivatives were synthesized by three-component reaction of aromatic aldehydes, 1,3-dicarbonyl compounds and hydroxylamine hydrochloride using triethylbenzylammonium chloride (TEBA) as the ca...N-Hydroxylacridinedione derivatives were synthesized by three-component reaction of aromatic aldehydes, 1,3-dicarbonyl compounds and hydroxylamine hydrochloride using triethylbenzylammonium chloride (TEBA) as the catalysis in water. The reaction has many advantages including good yields, easy to be separated and environmental friendliness.展开更多
A short and facile synthesis of a series of 1,2-dihydroquiazolin-4(3H)-ones was accomplished in good yields via novel reductive cyclization of o-nitrobenzamides with ketones promoted by TiCl4/Zn system. The structure ...A short and facile synthesis of a series of 1,2-dihydroquiazolin-4(3H)-ones was accomplished in good yields via novel reductive cyclization of o-nitrobenzamides with ketones promoted by TiCl4/Zn system. The structure was established on the basis of elemental analysis, IR, 1H NMR and confirmed by a single-crystal X-ray diffraction analysis. This method has the advantages of easily accessible starting materials, convenient manipulation and moderate to high yields.展开更多
The reaction of Schiff base and indole catalyzed by iodine in DMA, subsequently treated with DDQ, gave indolo[3,2-c]quinoline derivatives in good yields. The structure of 3e was confirmed by X-ray diffraction analysis.
基金Financially supported by the "Surpassing Project" Foundation of Jiangsu Province (No. QL9801) and Project of Scientific Research of Xuzhou Normal University (NO. 04XLA03)
文摘The title compound 2-amino-5,6-dihydro-4-(3,4-dimethoxyphenyl)-4H-benzo[h]- chromene-3-carbonitrile (C22H20N2O3, Mr = 360.40) was obtained by the reaction of 2-(3,4-dimeth- oxybenzylidene)-1-tetralone and malononitrile in DMF in the presence of KF-montmorillonite. Its structure was confirmed by IR and ^1H NMR spectra. The crystal is of monoclinic, space group C2/c with a = 24.101(6), b = 9.146(2), c = 17.238(3) ,A, β= 95.92(2)°, Z = 8, V= 3779.4(14) ,A^3, Dc = 1.267 g/cm^3, μ(MoKa) = 0.085 mm^-1, F(000) = 1520, R = 0.0409 and wR = 0.0981 for 2043 observed reflections (I 〉 2σ(I)).
基金This work was supported by the NNSFC (No. 20372057) Natural Science Foundation of Jiangsu Province (No. BK2001142)+2 种基金 the Open Foundation of Key Laboratory of Organic Synthesis of Jiangsu Province College of Chemistry and Chemical Engineering Su
文摘The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst under microwave irradiation. Its structure was charac- terized by X-ray single-crystal diffraction techniques with the following data: triclinic, space group P1, a = 5.4513(4), b = 7.619(1), c = 16.118(4) ?, α = 80.42(1), β = 83.43(1), γ = 79.29(1)°, V = 646.19(19) ?3, Mr = 280.70, μ(MoKα) = 0.301 mm-1, Z = 2 and Dc = 1.443 g/cm3. In the molecule the pyrimidine ring is of boat conformation.
基金This work was supported by the Natural Science Foundation of Jiangsu Education Department (No. 03KJB 150136)
文摘The title compound C35H30Br2O3 (C32H24Br2O2·CH3COCH3) has been synthesized by the dimerization of 2-(4'-bromobenzal)-1-indenone induced by low-valent titanium reagent, and characterized by elemental analysis, IR,^1H NMR and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.273(7), b = 11.036(7), c = 13.944(9) ,A°, a = 73.972(9), β =76.577(10),γ= 88.871(10)°, V = 1476.3(17)A°^3, Mr = 658.41, Z = 2, Dr = 1.481 g/cm^3, μ(MoKa) = 2.780 mm^-1, F(000) = 668, the final R = 0.0452 and wR = 0.0975. X-ray analysis reveals that the two cyclopentane rings spiro-fused each other adopt envelope conformations, while the other cyclopentane ring (C(1)--C(2)-C(7)-C(9)) is coplanar. In addition, there is a classical intermolecular hydrogen bond O(1)-H(1)...O(2) connecting the adjacent molecules into dimers.
基金This work was supported by the Education Committee Natural Science Foundation (No. 03KJB 150136).
文摘The title compound 1-(4-chlorophenyl)-2-cyano-3-amino-3a-hydroxy-3a,3b,6,7- tetrahydro-benzo[4,5]indene 2, has been synthesized by the reductive cyclization of 2-cyano-3- (4-chlorophenyl)-3-(1-tetralon-2-yl) propionitrile 1 induced by low-valent titanium reagent and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/c with a = 28.244(7), b = 14.401(3), c = 21.245(3)A,β= 115.71(2)°, V = 7786(3)A^3, Mr= 696.13, Dc = 1.188 g/cm^3, Z = 8,μ(MoKα) = 0.208 mm^-1, F(000) = 2916, R = 0.0783 and wR = 0.2350. X-ray analysis reveals that the five-membered ring (C(7)~C(l l)) adopts an envelop conformation, while the six-membered ring (C(10)~C(14), C(19)) has a half-chair conformation. Meanwhile, intermolecular H-bond interactions result in the formation of polymer.
基金ProjectsupportedbytheNaturalScienceFoundationofJiangsuProvince (No .BK2 0 0 114 2 )andtheNaturalScienceFoundationofJiang suEducationDepartment (No .0 1KJB15 0 0 0 8)andJiangsuProvinceKeyLaboratoryofChemical&EngineeringandTechnologyFounda tion (No .KJ
文摘A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation. This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3 carbonyl compound and urea. The structure of 4o was determined by single crystal X ray diffraction analysis.
文摘N-Hydroxylacridinedione derivatives were synthesized by three-component reaction of aromatic aldehydes, 1,3-dicarbonyl compounds and hydroxylamine hydrochloride using triethylbenzylammonium chloride (TEBA) as the catalysis in water. The reaction has many advantages including good yields, easy to be separated and environmental friendliness.
基金Project supported by the Natural Science Foundation of Education Committee of Jiangsu Province (No. 03KJB150136).
文摘A short and facile synthesis of a series of 1,2-dihydroquiazolin-4(3H)-ones was accomplished in good yields via novel reductive cyclization of o-nitrobenzamides with ketones promoted by TiCl4/Zn system. The structure was established on the basis of elemental analysis, IR, 1H NMR and confirmed by a single-crystal X-ray diffraction analysis. This method has the advantages of easily accessible starting materials, convenient manipulation and moderate to high yields.
基金We are grateful to the National Natural Science foundation of China,the Priority Academic Program Development of Jiangsu Higher Education Institutions,Qing Lan Project,College Industrialization Project (JHB2012-31) of Jiangsu Education Committee for financial support
文摘The reaction of Schiff base and indole catalyzed by iodine in DMA, subsequently treated with DDQ, gave indolo[3,2-c]quinoline derivatives in good yields. The structure of 3e was confirmed by X-ray diffraction analysis.