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 （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
The title compound 2 (C15H22NO4PS, Mr = 343.38) was prepared by the reaction of α-benzoylthioformmorpholine 1 with trimethyl phosphite. The crystal is of monoclinic, space group P21/c with a = 14.906(2), b = ...The title compound 2 (C15H22NO4PS, Mr = 343.38) was prepared by the reaction of α-benzoylthioformmorpholine 1 with trimethyl phosphite. The crystal is of monoclinic, space group P21/c with a = 14.906(2), b = 8.4711(12), c = 13.343(2) ?, β = 96.761(4)o, Z = 4, V = 1673.1(5) ?3, Dc = 1.363 g/cm3, μ(MoKα) = 3.06 cm-1, F(000) = 728, the final R = 0.0590 and wR = 0.1740 for 3036 observed reflections (I > 2σ(I)). X-ray analysis revealed that the interatomic distance of C(5)–C(6) is 1.353(4) ?, indicating it is a normal C=C double bond. The P(1) atom takes a distorted tetrahedral geometry, and the morpholine ring adopts a chair conformation. The morpholino group is located at the 1-position of vinylphosphonate, and the phenyl and thiomethyl groups at the 2-position.展开更多
The new title compound （2E,6E）-2,6-bis（2,3-dimethoxybenzylidene）cyclohexanone （C 24 H 26 O 5,M r=394.45） has been synthesized,and its crystal structure was studied.The title compound crystallizes in the orthorho...The new title compound （2E,6E）-2,6-bis（2,3-dimethoxybenzylidene）cyclohexanone （C 24 H 26 O 5,M r=394.45） has been synthesized,and its crystal structure was studied.The title compound crystallizes in the orthorhombic system,space group Pca2 1 with a=17.536（2）,b=14.8515（16）,c=8.0512（9）,V=2096.8（4） 3,Z=4,D c=1.250 g/cm 3,λ=0.71073,μ=0.087 mm-1 and F（000）=840.The structure was solved by direct methods and refined to R=0.0533 and wR=0.1248 from 2727 observed reflections （I 2σ（Ⅰ））.The title molecules are connected through hydrogen bonds to generate a 3-D supramolecule.The preliminary biological tests showed definitely biological activity for the title compound.展开更多
Two potential chiral auxiliaries, N (E ) enoyl(-) bornane 10,2 sultams, were synthesized from (-) bornane 10,2 sultams. The molecular crystal structures of the title compounds were determined by diffraction...Two potential chiral auxiliaries, N (E ) enoyl(-) bornane 10,2 sultams, were synthesized from (-) bornane 10,2 sultams. The molecular crystal structures of the title compounds were determined by diffraction analysis. The crystal of C 16 O 3SNH 25 belongs to a rhombic system, the space group is P 2 12 12 1 with cell parameters: a =0 734 6(7) nm, b =1 142 7(3) nm, c =2 009 7(3) nm, β =90 00°, V =1 686 9 nm 3, Z=4, D c=1 250 g/cm 3, μ =1 926 cm -1 and F (000)=672. The crystal of C 15 O 3SNH 23 belongs to a rhombic system, the space group is P 2 12 12 1 with cell parameters: a =0 738 2(2) nm, b =0 921 6(1) nm, c =2 280 9(8) nm, β =90 00°, V =1 551 7 nm 3, Z =4, D c=1 273 g/cm 3, μ =2 504 cm -1 and F (000)=640. The structural characteristics with respect to the potential utility for the stereoselective Michael addition reaction of the N enoyl group are discussed.展开更多
The title compound, （E）-1-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）- 3-（2-methoxyphenyl）-2-（1H-1,2,4-triazol-1-yl）propenol （3a）, was synthesized by the Aldol con- densation reaction of 1-（7-methox...The title compound, （E）-1-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）- 3-（2-methoxyphenyl）-2-（1H-1,2,4-triazol-1-yl）propenol （3a）, was synthesized by the Aldol con- densation reaction of 1-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）-2-（1,2,4-triazol- 1-yl）ethanone with 2-methoxybenzaldehyde and then reduced with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction： monoclinic system, space group P21 with a = 6.2002（3）, b = 12.8452（7）, c = 13.2257（7） ？, Z = 2, V = 1031.23（9） ？3, Mr = 407.46, Dc = 1.312 Mg/m3, S = 1.054, μ = 0.091 mm-1, F（000） = 432, the final R = 0.0353 and wR = 0.0769 for 3161 observed reflections （I 〉 2σ（I））. X-ray analysis displays that the title compound adopts an E configuration for the C（7）=C（8） double bond and S configuration for the chirality center with the specific rotation of –63.75°. Furthermore, the stability of the crystal was maintained through the intermolecular hydrogen bond O（1）–H？？？N（3）. The antitumor assay exhibits that the title compound 3a （E configuration） has a good antitumor activity against the Hela cell line with the IC50 value of 36.9 μM, which is better than that of 3b （Z configuration）.展开更多
The title compound tert-butyl 4-[（E）-4-（1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl）- 1-butenyl] benzoate has been synthesized and characterized by X-ray crystallography. It crystallizes in monoclinic, space group C2/c...The title compound tert-butyl 4-[（E）-4-（1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl）- 1-butenyl] benzoate has been synthesized and characterized by X-ray crystallography. It crystallizes in monoclinic, space group C2/c with a = 14.875（3）, b = 8.9796（13）, c = 34.736（6） A°, β = 95.981（4）°, V= 4614.4（14）A°^3, Z= 8, Dc = 1.213 g/cm^3, F（000） = 1792,μ（MoKα） = 0.084 mm^-1, R = 0.0602 and wR = 0.1445 for 4613 unique reflections with 2272 observed ones （I〉 2σ（I））. The results of crystal structure determination show that the title compound has a layer structure, and the two benzene rings in molecule are parallel to each other.展开更多
A new asymmetric bidentate copper（Ⅱ） complex,CuL 2（HL=2-（（E）-（4-bromophenylimino）methyl）-6-bromo-4-chlorophenol）,has been synthesized and characterized by elemental analyses and single-crystal X-ray diffrac...A new asymmetric bidentate copper（Ⅱ） complex,CuL 2（HL=2-（（E）-（4-bromophenylimino）methyl）-6-bromo-4-chlorophenol）,has been synthesized and characterized by elemental analyses and single-crystal X-ray diffraction.The complex crystallizes in the monoclinic space group P2 1 /c with a=11.218（3）,b=9.355（3）,c=13.449（4）,β=108.722（4）°,V=1336.8（6）3,Z=2,Dc=2.008 g/cm 3,μ（MoKα）=7.024 mm-1,F（000）=806,S=0.999,the final R=0.0342 and wR=0.0641for2611observed reflections （I〉2σ（I））.The central copper（Ⅱ） is four-coordinate and bonds to two nitrogen and two oxygen atoms from two Schiff base ligands.The complex is linked into a two-dimensional supramolecular structure by weak intermolecular interactions.In addition,DNA-binding properties of the metal complex were investigated using spectrometric titrations and viscosity measurements.The results show that the complex binds with calf-thymus DNA（CT-DNA）,presumably via a partial intercalative mode.The intrinsic binding constant of the Cu（Ⅱ） complex with DNA is 7.335×10 3 M-1.展开更多
2-Phenyl-3-thioformylindolizine and 1,2-dimethyl-3-thioformylindolizine undergo a novel desulfur coupling reaction in the presence of tributylphosphine to give （E）-1,2-bis（3-indolizinyl）ethenes in high yields. The...2-Phenyl-3-thioformylindolizine and 1,2-dimethyl-3-thioformylindolizine undergo a novel desulfur coupling reaction in the presence of tributylphosphine to give （E）-1,2-bis（3-indolizinyl）ethenes in high yields. The structures of products were confirmed by IR, ^1H NMR, MS, elemental analysis and single crystal X-ray diffraction analysis. The mechanisms involved in various stages of the reaction were discussed.展开更多
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.
基金The project was supported by the Key Laboratory of Organic Synthesis of Jiangsu Province (JSK016)
文摘The title compound 2 (C15H22NO4PS, Mr = 343.38) was prepared by the reaction of α-benzoylthioformmorpholine 1 with trimethyl phosphite. The crystal is of monoclinic, space group P21/c with a = 14.906(2), b = 8.4711(12), c = 13.343(2) ?, β = 96.761(4)o, Z = 4, V = 1673.1(5) ?3, Dc = 1.363 g/cm3, μ(MoKα) = 3.06 cm-1, F(000) = 728, the final R = 0.0590 and wR = 0.1740 for 3036 observed reflections (I > 2σ(I)). X-ray analysis revealed that the interatomic distance of C(5)–C(6) is 1.353(4) ?, indicating it is a normal C=C double bond. The P(1) atom takes a distorted tetrahedral geometry, and the morpholine ring adopts a chair conformation. The morpholino group is located at the 1-position of vinylphosphonate, and the phenyl and thiomethyl groups at the 2-position.
基金supported by the National Natural Science Foundation of China (81072683)Project of Wenzhou Sci & Tech Bureau (Y20100006)Natural Science Foundation of Zhejiang Province (Y20101108)
文摘The new title compound （2E,6E）-2,6-bis（2,3-dimethoxybenzylidene）cyclohexanone （C 24 H 26 O 5,M r=394.45） has been synthesized,and its crystal structure was studied.The title compound crystallizes in the orthorhombic system,space group Pca2 1 with a=17.536（2）,b=14.8515（16）,c=8.0512（9）,V=2096.8（4） 3,Z=4,D c=1.250 g/cm 3,λ=0.71073,μ=0.087 mm-1 and F（000）=840.The structure was solved by direct methods and refined to R=0.0533 and wR=0.1248 from 2727 observed reflections （I 2σ（Ⅰ））.The title molecules are connected through hydrogen bonds to generate a 3-D supramolecule.The preliminary biological tests showed definitely biological activity for the title compound.
文摘Two potential chiral auxiliaries, N (E ) enoyl(-) bornane 10,2 sultams, were synthesized from (-) bornane 10,2 sultams. The molecular crystal structures of the title compounds were determined by diffraction analysis. The crystal of C 16 O 3SNH 25 belongs to a rhombic system, the space group is P 2 12 12 1 with cell parameters: a =0 734 6(7) nm, b =1 142 7(3) nm, c =2 009 7(3) nm, β =90 00°, V =1 686 9 nm 3, Z=4, D c=1 250 g/cm 3, μ =1 926 cm -1 and F (000)=672. The crystal of C 15 O 3SNH 23 belongs to a rhombic system, the space group is P 2 12 12 1 with cell parameters: a =0 738 2(2) nm, b =0 921 6(1) nm, c =2 280 9(8) nm, β =90 00°, V =1 551 7 nm 3, Z =4, D c=1 273 g/cm 3, μ =2 504 cm -1 and F (000)=640. The structural characteristics with respect to the potential utility for the stereoselective Michael addition reaction of the N enoyl group are discussed.
基金Project supported by the National Natural Science Foundation of China(No.21442014)
文摘The title compound, （E）-1-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）- 3-（2-methoxyphenyl）-2-（1H-1,2,4-triazol-1-yl）propenol （3a）, was synthesized by the Aldol con- densation reaction of 1-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）-2-（1,2,4-triazol- 1-yl）ethanone with 2-methoxybenzaldehyde and then reduced with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction： monoclinic system, space group P21 with a = 6.2002（3）, b = 12.8452（7）, c = 13.2257（7） ？, Z = 2, V = 1031.23（9） ？3, Mr = 407.46, Dc = 1.312 Mg/m3, S = 1.054, μ = 0.091 mm-1, F（000） = 432, the final R = 0.0353 and wR = 0.0769 for 3161 observed reflections （I 〉 2σ（I））. X-ray analysis displays that the title compound adopts an E configuration for the C（7）=C（8） double bond and S configuration for the chirality center with the specific rotation of –63.75°. Furthermore, the stability of the crystal was maintained through the intermolecular hydrogen bond O（1）–H？？？N（3）. The antitumor assay exhibits that the title compound 3a （E configuration） has a good antitumor activity against the Hela cell line with the IC50 value of 36.9 μM, which is better than that of 3b （Z configuration）.
文摘The title compound tert-butyl 4-[（E）-4-（1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl）- 1-butenyl] benzoate has been synthesized and characterized by X-ray crystallography. It crystallizes in monoclinic, space group C2/c with a = 14.875（3）, b = 8.9796（13）, c = 34.736（6） A°, β = 95.981（4）°, V= 4614.4（14）A°^3, Z= 8, Dc = 1.213 g/cm^3, F（000） = 1792,μ（MoKα） = 0.084 mm^-1, R = 0.0602 and wR = 0.1445 for 4613 unique reflections with 2272 observed ones （I〉 2σ（I））. The results of crystal structure determination show that the title compound has a layer structure, and the two benzene rings in molecule are parallel to each other.
文摘A new asymmetric bidentate copper（Ⅱ） complex,CuL 2（HL=2-（（E）-（4-bromophenylimino）methyl）-6-bromo-4-chlorophenol）,has been synthesized and characterized by elemental analyses and single-crystal X-ray diffraction.The complex crystallizes in the monoclinic space group P2 1 /c with a=11.218（3）,b=9.355（3）,c=13.449（4）,β=108.722（4）°,V=1336.8（6）3,Z=2,Dc=2.008 g/cm 3,μ（MoKα）=7.024 mm-1,F（000）=806,S=0.999,the final R=0.0342 and wR=0.0641for2611observed reflections （I〉2σ（I））.The central copper（Ⅱ） is four-coordinate and bonds to two nitrogen and two oxygen atoms from two Schiff base ligands.The complex is linked into a two-dimensional supramolecular structure by weak intermolecular interactions.In addition,DNA-binding properties of the metal complex were investigated using spectrometric titrations and viscosity measurements.The results show that the complex binds with calf-thymus DNA（CT-DNA）,presumably via a partial intercalative mode.The intrinsic binding constant of the Cu（Ⅱ） complex with DNA is 7.335×10 3 M-1.
基金Project supported by the National Natural Science Foundation of China （No. 20672090）, the Natural Science Foundation of Jiangsu Education Department （No. 06KJD150015）, the Key Laboratory of Marine Biotechnology Foundation of Jiangsu Province （No. 2006HS014） and the Hualhai Institute of Technology Disciplinary Construction Foundation （No. XK200309）.
文摘2-Phenyl-3-thioformylindolizine and 1,2-dimethyl-3-thioformylindolizine undergo a novel desulfur coupling reaction in the presence of tributylphosphine to give （E）-1,2-bis（3-indolizinyl）ethenes in high yields. The structures of products were confirmed by IR, ^1H NMR, MS, elemental analysis and single crystal X-ray diffraction analysis. The mechanisms involved in various stages of the reaction were discussed.
