The title compound BBBT-Dry (C17H12Br2S5, Mr=536.42) has been synthesized and its structure feature has been described. BBBT-DTT is characterized by one dimensional chains formed by S…S (head to head) and Br…Br (tai...The title compound BBBT-Dry (C17H12Br2S5, Mr=536.42) has been synthesized and its structure feature has been described. BBBT-DTT is characterized by one dimensional chains formed by S…S (head to head) and Br…Br (tail to tail) intermolecular interactions.展开更多
New Schiff base Macrocyclic compound of 2,3: 11, 12:20, 21:29, 30-tetrabenzo-1,13,16,19,31,34-hexaoxa-5,6,8,9,23,24,26,27-octaaza-7,25-dithione-2,3:4,5:9,10:11,12:22, 23:27,28:29,30 cyclo-[36]ene (thione2B4[36] ene-O6...New Schiff base Macrocyclic compound of 2,3: 11, 12:20, 21:29, 30-tetrabenzo-1,13,16,19,31,34-hexaoxa-5,6,8,9,23,24,26,27-octaaza-7,25-dithione-2,3:4,5:9,10:11,12:22, 23:27,28:29,30 cyclo-[36]ene (thione2B4[36] ene-O6N8) containing THF has been prepared. It crystallizes in the monoclinic, space group P21/n. with parameters a=9.829(5) b=24.23(1), c=10.181(9), β=92.93(5)°, Z=2, V=2422(3)3, Dc=1.25gcm-3. Data collection: Rigaku AFC-5R diffractometer,(MoKα, λ=0.71069), ω /2θ scans. θmax=25°, empirical absorption correction, 4658 measured reflections, 4387 independent, 1743 observed reflections [I≥3σ(I)]. The final R=0.056. RW=0.069,S=1 .54, (Δ/σ)max=0.01,Δρmax=0.36e-3.展开更多
The treatment of 5 amino 1 (4 chlorophenyl) 1,2,3 triazol 4 carbohydrazide with equimolecular aryl isothiocyanate gave new derivatives 1 a—l . Twelve title compounds were obtained in 42% to 87% yields whe...The treatment of 5 amino 1 (4 chlorophenyl) 1,2,3 triazol 4 carbohydrazide with equimolecular aryl isothiocyanate gave new derivatives 1 a—l . Twelve title compounds were obtained in 42% to 87% yields when compounds 1 a—l were respectively treated with sodium hydroxide aqueous solution(2 mol/L). The products of Dimroth rearrangement were not observed in the experiment. The structures of all the compounds were confirmed by means of IR, 1H NMR, MS and elementary analysis.展开更多
Reactions of N,NA-diisopropyl-thiourea（abbreviated as L1） with CuC l2 and Cu Br2 afforded the trimeric（L1Cu Cl）3（1） and（L1Cu Br）3（2）, respectively, featuring the sulfur bridged Cu3S3 six-membered ring each a...Reactions of N,NA-diisopropyl-thiourea（abbreviated as L1） with CuC l2 and Cu Br2 afforded the trimeric（L1Cu Cl）3（1） and（L1Cu Br）3（2）, respectively, featuring the sulfur bridged Cu3S3 six-membered ring each as the core structure. During the reaction, Cu（Ⅱ） was reduced to Cu（I）. Similarly, the reactions of L1 with Cu Cl and Cu Br gave the same products as those by L1 with respective Cu Cl2 and Cu Br2. In contrast, treatment of 1,3-diisopropyl-4,5-dimethylimidazole-2（3H）-thione（L2） with Cu I led to the formation of sulfur and iodide mixed-bridged complex [（L2）4（Cu I）5]（3）, in which two co-vertice Cu3S2 I six-membered rings were fused by an iodide atom. Compounds obtained were characterized by 1H NMR and 13 C spectroscopy, elemental analysis, and single-crystal X-ray diffraction. 2 belongs to the monoclinic system, space group P21/c with a = 19.6009（10）, b = 11.5069（6）, c = 17.1744（9） A, β = 109.062（3）o, V = 3661.2（3） A3, C21H48Br3Cu3N6S3, Mr = 911.18, Z = 4, Dc = 1.653 Mg/m^3, μ（Mo Kα） = 5.192 mm–1, F（000） = 1824, S = 1.030, the final R = 0.0374 and w R = 0.0808 for 4988 observed reflections（I 2σ（I）） and R = 0.0726 and wR = 0.0916 for all data. 3·2THF belongs to the monoclinic system, space group I2/a with a = 19.7335（6）, b = 13.3544（4）, c = 29.6355（11） A, β = 105.415（2）o, V = 7528.9（4） A3, C52H96Cu5I5N8O2S4, Mr = 1945.81, Z = 4, Dc = 1.717 Mg/m^3, μ（Mo Kα） = 3.589 mm–1, F（000） = 3816, S = 1.034, the final R = 0.0325 and w R = 0.0810 for 5704 observed reflections（I 2σ（I）） and R = 0.0447 and wR = 0.0910 for all data.展开更多
A series of fluorine- and piperazine-containing 1,2,4-triazole thione derivatives were synthesized by the Mannich reaction of triazole intermediates with various substituted piperazines and formaldehyde in high yields...A series of fluorine- and piperazine-containing 1,2,4-triazole thione derivatives were synthesized by the Mannich reaction of triazole intermediates with various substituted piperazines and formaldehyde in high yields. Structures of title compounds were confirmed by melting points, IR,~1H NMR,^（13）C NMR and elemental analysis. The preliminary bioassays for 17 novel title compounds showed that several compounds have significant fungicidal activity against Cercospora arachidicola, Physalospora piricola and Rhizoctonia cerealis at 50 mg/m L.展开更多
Melamine trisulfonic acid（MTSA） can be used as an efficient and recyclable catalyst for the promotion of the synthesis of 3,4- dihydropyrimidin-2（1H）-ones/thiones（DHPMs） in the absence of solvent.All reactions w...Melamine trisulfonic acid（MTSA） can be used as an efficient and recyclable catalyst for the promotion of the synthesis of 3,4- dihydropyrimidin-2（1H）-ones/thiones（DHPMs） in the absence of solvent.All reactions were performed at 80℃in good to high yields.展开更多
A general and practical procedure for the syntheses of 3,4 dihydropyrimidine 2(1 H ) thiones by a one pot condensation of aldehyde, β ketoester or β diketone and thiourea using La (OTf) 3 as the catalyst ...A general and practical procedure for the syntheses of 3,4 dihydropyrimidine 2(1 H ) thiones by a one pot condensation of aldehyde, β ketoester or β diketone and thiourea using La (OTf) 3 as the catalyst is described. Mild reaction conditions, excellent yields as well as the environmentally friendly character of La(OTf) 3 make it an important alternative to the classic acid catalyzed Biginelli's reaction.展开更多
Synthesis of novel 4-（4-methylsulfonylphenyl）-3-phenyl-2（3H）-thiazole thione derivatives with functionalized diarylheterocycle pharmacophore as potential COX-2 inhibitors was described. The title compounds were sy...Synthesis of novel 4-（4-methylsulfonylphenyl）-3-phenyl-2（3H）-thiazole thione derivatives with functionalized diarylheterocycle pharmacophore as potential COX-2 inhibitors was described. The title compounds were synthesized by cyclocondensation of corresponding dithiocarbamate and 2-bromo-1-（4-methylsulfonylphenyl）ethanone, followed by dehydration with H2SO4. All of the target compounds were characterized by ^1H NMR, IR and mass spectral data.展开更多
Racemic R.S α arylethylamine was resolved by R（-）thiazolidine 2 thione 4 carboxylic acid, a new resolving agent abbreviated as , by which R（-）TTCA·S（-） arylethylamine salts 2a - 2e, 20 D= -47.24°\-64....Racemic R.S α arylethylamine was resolved by R（-）thiazolidine 2 thione 4 carboxylic acid, a new resolving agent abbreviated as , by which R（-）TTCA·S（-） arylethylamine salts 2a - 2e, 20 D= -47.24°\-64.40° and optically active R（+） α arylethylamines 3a - 3e , 74.54%\94.45% e.e., were obtained. Optically active S（-） α arylethylamines 4a - 4e , 72.84%\90.36% e.e., were obtained by the decomposition of 2a - 2e in basic solutions. The influence of substitutive group of the benzene ring on the basicity of the amino group was studied by semiempirical PM3 method. The structures of the R（-）TTCA·S（-） α phenylethylamine salt （2a（R S） configuration） and R（-）TTCA·R（+） α phenylethylamine salt （2a′（R R） configuration） have been established by means of X ray diffraction. They crystallize in a monoclinic system. Space group is P 2 l. The cell constants of 2a（R S） configuration were obtained as follows: a =1.387 8（2）, b =0.664 05（10）, c =1.580 0（2） nm; β =90 844（10）°, Z=4 ; those obtained for 2a′（R R） configuration were a= 1.080 6（2）, b =0.584 80（12）, c = 1.218 8（2） nm, β =110.38（3）°, V =0.722 0 nm 3, Z =2. There are intermolecular hydrogen bonds in the crystals of the two kinds of configurations of the amine salt. The hydrogen bond number in the unit cell of R（-）TTCA·S（-） α phenylethylamine salt is twice as much as that of R（-）TTCA·R（+） α phenylethylamine salt.展开更多
A new series of tetrahydropyrido[4,3-d]dihydropyrimidine-2-thiones （3a-3x） were designed and synthesized. Their structures were confirmed by 1H NMR, IR, MS and elemental analysis, and the conformation of compound 3j...A new series of tetrahydropyrido[4,3-d]dihydropyrimidine-2-thiones （3a-3x） were designed and synthesized. Their structures were confirmed by 1H NMR, IR, MS and elemental analysis, and the conformation of compound 3j was confirmed by X-ray diffraction. Preliminary bioassays indicated that most of the target compounds presented good antiproliferative activities against leukemic K562 cells, ovarian cancer HO-8910 cells and liver cancer SMMC-7721 cells in vitro. Among them the compounds 3i and 3m afford the best activity, the IC50 of them were 3.22 and 3.65 μg/mL against leukemic K562 cells, respectively, which were lower than the anticancer drug of clini- cal practice 5-FU （IC50 = 8.56μg/mL）. Preliminary mechanism of action studies revealed that compound 3i caused DNA fragmentation and activated caspase-3/7 in leukemic K562 cells.展开更多
The reaction of thiourea with p-methyl-β-p-chlorophenyl acrylophenone(1)is,in princi- ple,an attractive[3+ 3]-fragment approach to the synthesis of dihydropyrimidine bearing aryl groups.
Tradescantia Micronucleus(Trad-MCN)test was used toexamine the mutagenicity of drinking water and effect ofintervenient measure in the high incidence area of livercancer(Guangxi Fusui,China).The result showed that all...Tradescantia Micronucleus(Trad-MCN)test was used toexamine the mutagenicity of drinking water and effect ofintervenient measure in the high incidence area of livercancer(Guangxi Fusui,China).The result showed that allthe river samples and tap samples mere negative while 28out of 29 pond samples and shallow well samples展开更多
Curcumin 3,4-dihydropyrimidinones/thiones/imines have been synthesized using one-pot cyclocondensation of curcumin with substituted aromatic aldehydes and urea/thiourea/guanidine in the presence of chitosamine hydroch...Curcumin 3,4-dihydropyrimidinones/thiones/imines have been synthesized using one-pot cyclocondensation of curcumin with substituted aromatic aldehydes and urea/thiourea/guanidine in the presence of chitosamine hydrochloride as a biodegradable and nontoxic catalyst under solvent-free microwave irradiation.The synthesized product was purified by crystallization from ethanol and the process does not involve any hazardous solvent.All the synthesized curcumin derivatives 4a-o were screened for antioxidant and anti-inflammatory activity.Biological activity data of the synthesized showed that most of the synthesized compounds exhibited greater antioxidant and anti-inflammatory activity than curcumin.展开更多
文摘The title compound BBBT-Dry (C17H12Br2S5, Mr=536.42) has been synthesized and its structure feature has been described. BBBT-DTT is characterized by one dimensional chains formed by S…S (head to head) and Br…Br (tail to tail) intermolecular interactions.
文摘New Schiff base Macrocyclic compound of 2,3: 11, 12:20, 21:29, 30-tetrabenzo-1,13,16,19,31,34-hexaoxa-5,6,8,9,23,24,26,27-octaaza-7,25-dithione-2,3:4,5:9,10:11,12:22, 23:27,28:29,30 cyclo-[36]ene (thione2B4[36] ene-O6N8) containing THF has been prepared. It crystallizes in the monoclinic, space group P21/n. with parameters a=9.829(5) b=24.23(1), c=10.181(9), β=92.93(5)°, Z=2, V=2422(3)3, Dc=1.25gcm-3. Data collection: Rigaku AFC-5R diffractometer,(MoKα, λ=0.71069), ω /2θ scans. θmax=25°, empirical absorption correction, 4658 measured reflections, 4387 independent, 1743 observed reflections [I≥3σ(I)]. The final R=0.056. RW=0.069,S=1 .54, (Δ/σ)max=0.01,Δρmax=0.36e-3.
文摘The treatment of 5 amino 1 (4 chlorophenyl) 1,2,3 triazol 4 carbohydrazide with equimolecular aryl isothiocyanate gave new derivatives 1 a—l . Twelve title compounds were obtained in 42% to 87% yields when compounds 1 a—l were respectively treated with sodium hydroxide aqueous solution(2 mol/L). The products of Dimroth rearrangement were not observed in the experiment. The structures of all the compounds were confirmed by means of IR, 1H NMR, MS and elementary analysis.
基金supported by the Research Fund for Teachers of Central South University(2013JSJJ007)the Science and Technology Planning Project of Hunan Province(2013FJ2003)
文摘Reactions of N,NA-diisopropyl-thiourea（abbreviated as L1） with CuC l2 and Cu Br2 afforded the trimeric（L1Cu Cl）3（1） and（L1Cu Br）3（2）, respectively, featuring the sulfur bridged Cu3S3 six-membered ring each as the core structure. During the reaction, Cu（Ⅱ） was reduced to Cu（I）. Similarly, the reactions of L1 with Cu Cl and Cu Br gave the same products as those by L1 with respective Cu Cl2 and Cu Br2. In contrast, treatment of 1,3-diisopropyl-4,5-dimethylimidazole-2（3H）-thione（L2） with Cu I led to the formation of sulfur and iodide mixed-bridged complex [（L2）4（Cu I）5]（3）, in which two co-vertice Cu3S2 I six-membered rings were fused by an iodide atom. Compounds obtained were characterized by 1H NMR and 13 C spectroscopy, elemental analysis, and single-crystal X-ray diffraction. 2 belongs to the monoclinic system, space group P21/c with a = 19.6009（10）, b = 11.5069（6）, c = 17.1744（9） A, β = 109.062（3）o, V = 3661.2（3） A3, C21H48Br3Cu3N6S3, Mr = 911.18, Z = 4, Dc = 1.653 Mg/m^3, μ（Mo Kα） = 5.192 mm–1, F（000） = 1824, S = 1.030, the final R = 0.0374 and w R = 0.0808 for 4988 observed reflections（I 2σ（I）） and R = 0.0726 and wR = 0.0916 for all data. 3·2THF belongs to the monoclinic system, space group I2/a with a = 19.7335（6）, b = 13.3544（4）, c = 29.6355（11） A, β = 105.415（2）o, V = 7528.9（4） A3, C52H96Cu5I5N8O2S4, Mr = 1945.81, Z = 4, Dc = 1.717 Mg/m^3, μ（Mo Kα） = 3.589 mm–1, F（000） = 3816, S = 1.034, the final R = 0.0325 and w R = 0.0810 for 5704 observed reflections（I 2σ（I）） and R = 0.0447 and wR = 0.0910 for all data.
基金supported by the National Natural Science Foundation of China (No. 21372133)‘‘111’’ Project of Ministry of Education of China (No. B06005)
文摘A series of fluorine- and piperazine-containing 1,2,4-triazole thione derivatives were synthesized by the Mannich reaction of triazole intermediates with various substituted piperazines and formaldehyde in high yields. Structures of title compounds were confirmed by melting points, IR,~1H NMR,^（13）C NMR and elemental analysis. The preliminary bioassays for 17 novel title compounds showed that several compounds have significant fungicidal activity against Cercospora arachidicola, Physalospora piricola and Rhizoctonia cerealis at 50 mg/m L.
基金the University of Guilan Research Council for the partial support of this work
文摘Melamine trisulfonic acid（MTSA） can be used as an efficient and recyclable catalyst for the promotion of the synthesis of 3,4- dihydropyrimidin-2（1H）-ones/thiones（DHPMs） in the absence of solvent.All reactions were performed at 80℃in good to high yields.
文摘A general and practical procedure for the syntheses of 3,4 dihydropyrimidine 2(1 H ) thiones by a one pot condensation of aldehyde, β ketoester or β diketone and thiourea using La (OTf) 3 as the catalyst is described. Mild reaction conditions, excellent yields as well as the environmentally friendly character of La(OTf) 3 make it an important alternative to the classic acid catalyzed Biginelli's reaction.
文摘Synthesis of novel 4-（4-methylsulfonylphenyl）-3-phenyl-2（3H）-thiazole thione derivatives with functionalized diarylheterocycle pharmacophore as potential COX-2 inhibitors was described. The title compounds were synthesized by cyclocondensation of corresponding dithiocarbamate and 2-bromo-1-（4-methylsulfonylphenyl）ethanone, followed by dehydration with H2SO4. All of the target compounds were characterized by ^1H NMR, IR and mass spectral data.
文摘Racemic R.S α arylethylamine was resolved by R（-）thiazolidine 2 thione 4 carboxylic acid, a new resolving agent abbreviated as , by which R（-）TTCA·S（-） arylethylamine salts 2a - 2e, 20 D= -47.24°\-64.40° and optically active R（+） α arylethylamines 3a - 3e , 74.54%\94.45% e.e., were obtained. Optically active S（-） α arylethylamines 4a - 4e , 72.84%\90.36% e.e., were obtained by the decomposition of 2a - 2e in basic solutions. The influence of substitutive group of the benzene ring on the basicity of the amino group was studied by semiempirical PM3 method. The structures of the R（-）TTCA·S（-） α phenylethylamine salt （2a（R S） configuration） and R（-）TTCA·R（+） α phenylethylamine salt （2a′（R R） configuration） have been established by means of X ray diffraction. They crystallize in a monoclinic system. Space group is P 2 l. The cell constants of 2a（R S） configuration were obtained as follows: a =1.387 8（2）, b =0.664 05（10）, c =1.580 0（2） nm; β =90 844（10）°, Z=4 ; those obtained for 2a′（R R） configuration were a= 1.080 6（2）, b =0.584 80（12）, c = 1.218 8（2） nm, β =110.38（3）°, V =0.722 0 nm 3, Z =2. There are intermolecular hydrogen bonds in the crystals of the two kinds of configurations of the amine salt. The hydrogen bond number in the unit cell of R（-）TTCA·S（-） α phenylethylamine salt is twice as much as that of R（-）TTCA·R（+） α phenylethylamine salt.
文摘A new series of tetrahydropyrido[4,3-d]dihydropyrimidine-2-thiones （3a-3x） were designed and synthesized. Their structures were confirmed by 1H NMR, IR, MS and elemental analysis, and the conformation of compound 3j was confirmed by X-ray diffraction. Preliminary bioassays indicated that most of the target compounds presented good antiproliferative activities against leukemic K562 cells, ovarian cancer HO-8910 cells and liver cancer SMMC-7721 cells in vitro. Among them the compounds 3i and 3m afford the best activity, the IC50 of them were 3.22 and 3.65 μg/mL against leukemic K562 cells, respectively, which were lower than the anticancer drug of clini- cal practice 5-FU （IC50 = 8.56μg/mL）. Preliminary mechanism of action studies revealed that compound 3i caused DNA fragmentation and activated caspase-3/7 in leukemic K562 cells.
文摘The reaction of thiourea with p-methyl-β-p-chlorophenyl acrylophenone(1)is,in princi- ple,an attractive[3+ 3]-fragment approach to the synthesis of dihydropyrimidine bearing aryl groups.
文摘Tradescantia Micronucleus(Trad-MCN)test was used toexamine the mutagenicity of drinking water and effect ofintervenient measure in the high incidence area of livercancer(Guangxi Fusui,China).The result showed that allthe river samples and tap samples mere negative while 28out of 29 pond samples and shallow well samples
基金the Madhya Pradesh Council of Science and Technology, Bhopal, India for financial support (No. 4468/CST/R&D/2010)
文摘Curcumin 3,4-dihydropyrimidinones/thiones/imines have been synthesized using one-pot cyclocondensation of curcumin with substituted aromatic aldehydes and urea/thiourea/guanidine in the presence of chitosamine hydrochloride as a biodegradable and nontoxic catalyst under solvent-free microwave irradiation.The synthesized product was purified by crystallization from ethanol and the process does not involve any hazardous solvent.All the synthesized curcumin derivatives 4a-o were screened for antioxidant and anti-inflammatory activity.Biological activity data of the synthesized showed that most of the synthesized compounds exhibited greater antioxidant and anti-inflammatory activity than curcumin.
