Cyclodextrins have gained wide attentions for their unique physicochemicai properties. In recent years, conducting polymers with special micro-structure and properties are synthesized in the presence of cyclodextrins....Cyclodextrins have gained wide attentions for their unique physicochemicai properties. In recent years, conducting polymers with special micro-structure and properties are synthesized in the presence of cyclodextrins. In this article, the application of cyclodextrins in the synthesis process of conducting polymer metarials is discussed. And authors' study results are summarized.展开更多
Some new 2-thioxo thiazole, 2-thioxo 1,3,4- thiadiazole and 3-thioxo-1,3,4-triazole derivatives (3-17) have been synthesized through ring closure reactions ofdithioic formic acid hydrazones 2 with functional reagent...Some new 2-thioxo thiazole, 2-thioxo 1,3,4- thiadiazole and 3-thioxo-1,3,4-triazole derivatives (3-17) have been synthesized through ring closure reactions ofdithioic formic acid hydrazones 2 with functional reagents in different medium. Former structures of the products have been established by the help of elemental and spectral analysis. Most of the obtained targets showed a moderate activity towards some microbes in comparison with two antibiotics Pipercillin and Mycostatine.展开更多
Some more new sulfur compounds bearing heterocyclic systems mainly 2-thioxo-1,3,4-thiadiazinone derivatives 2-7 and 3-thioxo-1,2,4-triazole derivatives 9 have been synthetic via alkylation, acylation and condensation ...Some more new sulfur compounds bearing heterocyclic systems mainly 2-thioxo-1,3,4-thiadiazinone derivatives 2-7 and 3-thioxo-1,2,4-triazole derivatives 9 have been synthetic via alkylation, acylation and condensation of dithioic formic acid hydrazide 1 through ring closure reactions with α,β-bi functional groups compounds. Most of the obtained target showed a highly activity towards some microbial in compare with two references antibiotics, Pipercillin and Mycostatine. The structures of the products have been established from their elemental and spectral analysis.展开更多
Photolysis rate (J1) and reaction rate constants (kl) for the biacetyl (butane-2,3-dione) were evaluated in aqueous phase using a continuous photolysis system with a conventional Xe-Hg arc lamp as a light source...Photolysis rate (J1) and reaction rate constants (kl) for the biacetyl (butane-2,3-dione) were evaluated in aqueous phase using a continuous photolysis system with a conventional Xe-Hg arc lamp as a light source. The OH radicals was generated by H2OE/UV process and biacetyl (CH3C(O)C(O)CH3) concentrations were monitored using 2,4-DNPH derivatization method. 2,3-butanedione molecule is widely present in the atmosphere, it have been detected in hydrometeors (fogs, rain, and clouds) and at a significant yield (up to 10μmolar). The measurements were performed at 294 K and with free pH values. Our results lead to the following obtained values: J1= 3×10^-4 S^-1 and k1 = (6.17±0.95)×10^8 M^-1·s^-1.The uncertainty listed above is ±15%.展开更多
As benzoxazin-4-ones and quinazolines linked to indole nucleus acting as a good pharmacophore, the synthesis of these compounds has significant meaning. The key intermediates 2-(2', 5'-disubstituted-indol-2'-yl...As benzoxazin-4-ones and quinazolines linked to indole nucleus acting as a good pharmacophore, the synthesis of these compounds has significant meaning. The key intermediates 2-(2', 5'-disubstituted-indol-2'-yl)-4H-3, 1-benzoxazin-4-ones (3) were synthesized from cyclocondensation of indole-2-carbonyl chlorides (2) and anthranilic acid. Compound (3) on reaction with thiosemicarbazide and o-phenylene diamine afforded the compound (4) and (6) respectively. Compound (4) subjected to intramolecular cyclization under thermal conditions above its melting point afforded the compound (5). Similarly compound (3) on fusion with o- phenylene diamine gave compound (7). Structures of these compounds were confirmed by their spectral studies. The compounds were screened for their antimicrobial activity and the results were reported.展开更多
Diisopropylidenated α-D-glucofuranose (1) was oxidated with CrO3-pyridine complex. Oxidated product and its hydrate were separated and were reduced together to synthesize diisopropylidenated α-D-allofuranose ( 3...Diisopropylidenated α-D-glucofuranose (1) was oxidated with CrO3-pyridine complex. Oxidated product and its hydrate were separated and were reduced together to synthesize diisopropylidenated α-D-allofuranose ( 3). The yield of 3 increased by 8% than that with only oxidated product as reduction substrate. Benzoylated derivative of 3 was selectively nydrolyzed and dimesylated to synthesize 3-O-benzoyl-1 .2- O- isopropylidene-α-D-allofuranose ( 5 ) and its dimesylated derivative respectively. The overall yield of 5 from 1 was 36%. Each step and final products were analyzed by ^1H-NMR spectra and other methods. The experiments showed that the influence of acetic acid concentration on selective hydrolysis was obvious. The hydrolysis yield was 81.8%. Oxidation. reduction and other procedures were practical and had application potential.展开更多
A series of novel pyrazoles compounds were synthesized by the reaction of five kinds of substitute α-bromoacetophenone with pyrazole intermediates which was prepared by the reaction of chalcones and thiosemicarbazone...A series of novel pyrazoles compounds were synthesized by the reaction of five kinds of substitute α-bromoacetophenone with pyrazole intermediates which was prepared by the reaction of chalcones and thiosemicarbazones. This method has some advantages such as mild reaction condition, easy operation and higher yield. All the compounds were confirmed by elemental analysis, IR and 1H NMR.展开更多
The first successful attempt to prepare W_3S_4 {S_2P (OEt )_2}_4(H_2O) in organic phase is reported. Its substitution and addition reactions are investigated systematically, and the substitution sequences of the '...The first successful attempt to prepare W_3S_4 {S_2P (OEt )_2}_4(H_2O) in organic phase is reported. Its substitution and addition reactions are investigated systematically, and the substitution sequences of the 'loose' ligands are determined. The crystallographic data of the cluster compounds with [W_3S_4] ̄(4+) and [W_3CuS_4] ̄(5+) cores are compared and their UV-Vis spectra are firstly reported. Thus, the 'quasi-aromaticity' of the [W_3S_4] ̄(4+) core of these cluster compounds is discussed.展开更多
A novel tandem reductive amination/intermolecular nucleophilic aromatic substitution (SNAr) sequence has been established for the synthesis of amine containing pyrimidine in formation of one carbon-oxygen and one carb...A novel tandem reductive amination/intermolecular nucleophilic aromatic substitution (SNAr) sequence has been established for the synthesis of amine containing pyrimidine in formation of one carbon-oxygen and one carbon-nitrogen bonds in a one-pot fashion. Treatment of aldehyde with arylamine, 2-methanesulfonyl-4,6-dimeth-oxypyrimidine and sodium borohydride provides good overall yield. The p-toluenesulfonic acid (PTSA) can be used as activator and is generally needed in the reaction. Dioxane is the preferred reaction solvent, but reactions can also be carried out in tetrahydrofuran (THF), MeCN, toluene and dichloromethane. The procedure is carried out effectively in the presence of K2CO3. The reaction proceeds smoothly with aromatic aldehydes and arylamines possessing elec-tron-donating or-withdrawing groups. This method can be applied to the synthesis of the oilseed rape herbicide and is superior to the classical one in several aspects: cutting out several purification steps, minimizing solvent use and chemical waste, and saving time. Its advantages such as operational convenience, high-efficient synthesis, and starting material availability make it a desirable method for preparing amines with molecular diversity and biological activity.展开更多
A novel series of benzimidazole derived naphthalimide triazoles and some corresponding triazoliums have been successfully synthesized and characterized by 1H NMR, 13 C NMR, 1H-1H COSY, IR and HRMS spectra. All the new...A novel series of benzimidazole derived naphthalimide triazoles and some corresponding triazoliums have been successfully synthesized and characterized by 1H NMR, 13 C NMR, 1H-1H COSY, IR and HRMS spectra. All the new compounds were screened for their antimicrobial activities in vitro by two-fold serial dilution. 2-Chlorobenzyl triazolium 8g and compound 9b with octyl group exhibited the best antibacterial activities among all the tested compounds, especially against S. aureus with inhibitory concentration of 2 μg/mL which was equipotent potency to Norfloxacin(MIC=2 μg/mL) and more active than Chloromycin(MIC=7 μg/mL). Triazoliums 8g and 8f bearing 3-fluorobenzyl moiety displayed the best antifungal activities(MIC=2-19 μg/mL) against all the tested fungal strains without being toxic to PC12 cell line within concentration of 128 μg/m L. Further investigations by fluorescence and UV-Vis spectroscopic methods revealed that the compound 8g could effectively intercalate into calf thymus DNA to form the 8g-DNA complex which could block DNA replication, exerting powerful antimicrobial activities.展开更多
The cationic reagent 1-(3-aminopropyl)-3-butylimidazolium bromide(BAPI) was exploited for the derivatization of carboxyl groups on peptides.Nearly 100% derivatization efficiency was achieved with the synthetic peptide...The cationic reagent 1-(3-aminopropyl)-3-butylimidazolium bromide(BAPI) was exploited for the derivatization of carboxyl groups on peptides.Nearly 100% derivatization efficiency was achieved with the synthetic peptide RVYVHPI(RI-7).Furthermore,the peptide derivative was stable in a 0.1% TFA/water solution or a 0.1%(v/v) TFA/acetonitrile/water solution for at least one week.The effect of BAPI derivatization on the ionization of the peptide RI-7 was further investigated,and the detection sensitivity was improved >42-fold via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry(MALDI-TOF MS),thus outperforming the commercial piperazine derivatization approach.Moreover,the charge states of the peptide were largely increased via BAPI derivatization by electrospray ionization(ESI) MS.The results indicate the potential merits of BAPI derivatization for high sensitivity peptide analysis by MS.展开更多
Caffeine is one of methyl xanthine compounds,which has the similar mode of action as ryanodine receptor insecticide.In order to find novel and efficient insecticide,structural modification of certain methyl xanthine c...Caffeine is one of methyl xanthine compounds,which has the similar mode of action as ryanodine receptor insecticide.In order to find novel and efficient insecticide,structural modification of certain methyl xanthine compounds was made by introducing some common pesticidal active moieties into the structure of caffeine.Eleven novel methyl xanthine compounds were synthesized and characterized by 1H nuclear magnetic resonance(1H NMR),elemental analylsis or high-resolution mass spectrometry(HRMS).According to the biological activity results,it was found that these new compounds show moderate activity towards Mythimna separata Walker and Culex pipiens pallens.For example,compound 2d shows a lethality rate of 40% at 200 mg/L towards Mythimna separata Walker,compounds 2i and 2f show 56.7% and 53.3% lethality rates at 2 mg/L towards Culex pipiens pallens,which are all better than caffeine.In addition,some compounds of them show moderate antifungal activity to some plant pathogenous fungi.展开更多
文摘Cyclodextrins have gained wide attentions for their unique physicochemicai properties. In recent years, conducting polymers with special micro-structure and properties are synthesized in the presence of cyclodextrins. In this article, the application of cyclodextrins in the synthesis process of conducting polymer metarials is discussed. And authors' study results are summarized.
文摘Some new 2-thioxo thiazole, 2-thioxo 1,3,4- thiadiazole and 3-thioxo-1,3,4-triazole derivatives (3-17) have been synthesized through ring closure reactions ofdithioic formic acid hydrazones 2 with functional reagents in different medium. Former structures of the products have been established by the help of elemental and spectral analysis. Most of the obtained targets showed a moderate activity towards some microbes in comparison with two antibiotics Pipercillin and Mycostatine.
文摘Some more new sulfur compounds bearing heterocyclic systems mainly 2-thioxo-1,3,4-thiadiazinone derivatives 2-7 and 3-thioxo-1,2,4-triazole derivatives 9 have been synthetic via alkylation, acylation and condensation of dithioic formic acid hydrazide 1 through ring closure reactions with α,β-bi functional groups compounds. Most of the obtained target showed a highly activity towards some microbial in compare with two references antibiotics, Pipercillin and Mycostatine. The structures of the products have been established from their elemental and spectral analysis.
文摘Photolysis rate (J1) and reaction rate constants (kl) for the biacetyl (butane-2,3-dione) were evaluated in aqueous phase using a continuous photolysis system with a conventional Xe-Hg arc lamp as a light source. The OH radicals was generated by H2OE/UV process and biacetyl (CH3C(O)C(O)CH3) concentrations were monitored using 2,4-DNPH derivatization method. 2,3-butanedione molecule is widely present in the atmosphere, it have been detected in hydrometeors (fogs, rain, and clouds) and at a significant yield (up to 10μmolar). The measurements were performed at 294 K and with free pH values. Our results lead to the following obtained values: J1= 3×10^-4 S^-1 and k1 = (6.17±0.95)×10^8 M^-1·s^-1.The uncertainty listed above is ±15%.
文摘As benzoxazin-4-ones and quinazolines linked to indole nucleus acting as a good pharmacophore, the synthesis of these compounds has significant meaning. The key intermediates 2-(2', 5'-disubstituted-indol-2'-yl)-4H-3, 1-benzoxazin-4-ones (3) were synthesized from cyclocondensation of indole-2-carbonyl chlorides (2) and anthranilic acid. Compound (3) on reaction with thiosemicarbazide and o-phenylene diamine afforded the compound (4) and (6) respectively. Compound (4) subjected to intramolecular cyclization under thermal conditions above its melting point afforded the compound (5). Similarly compound (3) on fusion with o- phenylene diamine gave compound (7). Structures of these compounds were confirmed by their spectral studies. The compounds were screened for their antimicrobial activity and the results were reported.
基金Supported by Tianjin Natural Science Foundation ( No. 05YFJMJC09600).
文摘Diisopropylidenated α-D-glucofuranose (1) was oxidated with CrO3-pyridine complex. Oxidated product and its hydrate were separated and were reduced together to synthesize diisopropylidenated α-D-allofuranose ( 3). The yield of 3 increased by 8% than that with only oxidated product as reduction substrate. Benzoylated derivative of 3 was selectively nydrolyzed and dimesylated to synthesize 3-O-benzoyl-1 .2- O- isopropylidene-α-D-allofuranose ( 5 ) and its dimesylated derivative respectively. The overall yield of 5 from 1 was 36%. Each step and final products were analyzed by ^1H-NMR spectra and other methods. The experiments showed that the influence of acetic acid concentration on selective hydrolysis was obvious. The hydrolysis yield was 81.8%. Oxidation. reduction and other procedures were practical and had application potential.
基金The authors are extremely grateful to the National Nature Science Foundation of China for supporting this research (No.20962018, No20862015, No.20762009 and No.20562011).
文摘A series of novel pyrazoles compounds were synthesized by the reaction of five kinds of substitute α-bromoacetophenone with pyrazole intermediates which was prepared by the reaction of chalcones and thiosemicarbazones. This method has some advantages such as mild reaction condition, easy operation and higher yield. All the compounds were confirmed by elemental analysis, IR and 1H NMR.
文摘The first successful attempt to prepare W_3S_4 {S_2P (OEt )_2}_4(H_2O) in organic phase is reported. Its substitution and addition reactions are investigated systematically, and the substitution sequences of the 'loose' ligands are determined. The crystallographic data of the cluster compounds with [W_3S_4] ̄(4+) and [W_3CuS_4] ̄(5+) cores are compared and their UV-Vis spectra are firstly reported. Thus, the 'quasi-aromaticity' of the [W_3S_4] ̄(4+) core of these cluster compounds is discussed.
基金Project (Nos. Y407118 and D3080282) supported by the Natural Science Foundation of Zhejiang Province, China
文摘A novel tandem reductive amination/intermolecular nucleophilic aromatic substitution (SNAr) sequence has been established for the synthesis of amine containing pyrimidine in formation of one carbon-oxygen and one carbon-nitrogen bonds in a one-pot fashion. Treatment of aldehyde with arylamine, 2-methanesulfonyl-4,6-dimeth-oxypyrimidine and sodium borohydride provides good overall yield. The p-toluenesulfonic acid (PTSA) can be used as activator and is generally needed in the reaction. Dioxane is the preferred reaction solvent, but reactions can also be carried out in tetrahydrofuran (THF), MeCN, toluene and dichloromethane. The procedure is carried out effectively in the presence of K2CO3. The reaction proceeds smoothly with aromatic aldehydes and arylamines possessing elec-tron-donating or-withdrawing groups. This method can be applied to the synthesis of the oilseed rape herbicide and is superior to the classical one in several aspects: cutting out several purification steps, minimizing solvent use and chemical waste, and saving time. Its advantages such as operational convenience, high-efficient synthesis, and starting material availability make it a desirable method for preparing amines with molecular diversity and biological activity.
基金supported by the National Natural Science Foundation of China(21172181,21372186,81450110094)the key program from Natural Science Foundation of Chongqing(CSTC2012jj B10026)+3 种基金the Specialized Research Fund for the Doctoral Program of Higher Education of China(SRFDP 20110182110007)the Doctoral Fund of Southwest University(SWU111075)the Research Funds for the Central Universities(XDJK2013C112)Chongqing Special Foundation for Postdoctoral Research Proposal(Xm201450)
文摘A novel series of benzimidazole derived naphthalimide triazoles and some corresponding triazoliums have been successfully synthesized and characterized by 1H NMR, 13 C NMR, 1H-1H COSY, IR and HRMS spectra. All the new compounds were screened for their antimicrobial activities in vitro by two-fold serial dilution. 2-Chlorobenzyl triazolium 8g and compound 9b with octyl group exhibited the best antibacterial activities among all the tested compounds, especially against S. aureus with inhibitory concentration of 2 μg/mL which was equipotent potency to Norfloxacin(MIC=2 μg/mL) and more active than Chloromycin(MIC=7 μg/mL). Triazoliums 8g and 8f bearing 3-fluorobenzyl moiety displayed the best antifungal activities(MIC=2-19 μg/mL) against all the tested fungal strains without being toxic to PC12 cell line within concentration of 128 μg/m L. Further investigations by fluorescence and UV-Vis spectroscopic methods revealed that the compound 8g could effectively intercalate into calf thymus DNA to form the 8g-DNA complex which could block DNA replication, exerting powerful antimicrobial activities.
基金supported by National Basic Research Program of China (2012CB910604)National Natural Science Foundation of China (21205027,21005079,20935004)+1 种基金Analytical Method Innovation Program of Ministry of Science and Technology of China (2010IM030500)Natural Science Foundation of Hebei Province (B2012201095)
文摘The cationic reagent 1-(3-aminopropyl)-3-butylimidazolium bromide(BAPI) was exploited for the derivatization of carboxyl groups on peptides.Nearly 100% derivatization efficiency was achieved with the synthetic peptide RVYVHPI(RI-7).Furthermore,the peptide derivative was stable in a 0.1% TFA/water solution or a 0.1%(v/v) TFA/acetonitrile/water solution for at least one week.The effect of BAPI derivatization on the ionization of the peptide RI-7 was further investigated,and the detection sensitivity was improved >42-fold via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry(MALDI-TOF MS),thus outperforming the commercial piperazine derivatization approach.Moreover,the charge states of the peptide were largely increased via BAPI derivatization by electrospray ionization(ESI) MS.The results indicate the potential merits of BAPI derivatization for high sensitivity peptide analysis by MS.
基金Supported by the National Basic Research Program of China(No.2010CB126106), the National Natural Science Foundation of China(Nos.21272129, 21372133), the National Key Technologies Research and Development Program, China(No. 2011BAE06B05-3) and Specialized Research Fund for the Doctorial Program of Higher Education, China(No.20110031110017).
文摘Caffeine is one of methyl xanthine compounds,which has the similar mode of action as ryanodine receptor insecticide.In order to find novel and efficient insecticide,structural modification of certain methyl xanthine compounds was made by introducing some common pesticidal active moieties into the structure of caffeine.Eleven novel methyl xanthine compounds were synthesized and characterized by 1H nuclear magnetic resonance(1H NMR),elemental analylsis or high-resolution mass spectrometry(HRMS).According to the biological activity results,it was found that these new compounds show moderate activity towards Mythimna separata Walker and Culex pipiens pallens.For example,compound 2d shows a lethality rate of 40% at 200 mg/L towards Mythimna separata Walker,compounds 2i and 2f show 56.7% and 53.3% lethality rates at 2 mg/L towards Culex pipiens pallens,which are all better than caffeine.In addition,some compounds of them show moderate antifungal activity to some plant pathogenous fungi.