Thiazine sugar derivative 2 was synthesized and characterized by IR, NMR and H RMS, and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system （C16H24N2O8S2, Mr = 436...Thiazine sugar derivative 2 was synthesized and characterized by IR, NMR and H RMS, and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system （C16H24N2O8S2, Mr = 436.49） with space group P21, a = 10.311（2）, b = 9.1198（18）, c = 11.623（2）A, β = 109.47（3）°, V= 1030.4（4）A^3, Z= 2, Dc = 1.407 g/cm^3, F（000）= 460, μ= 0.303 mm^-1, the final R = 0.0437 and wR = 0.0561 for 1954 observed reflections （I 〉 2σ（I））. Nine hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparison with the original material.展开更多
A series of novel multithioether derivatives were synthesized by the combination of thiazoline and thiazine with dibro- mides and their structures were characterized by IR, 1H NMR, MS and elemental analysis. The synth...A series of novel multithioether derivatives were synthesized by the combination of thiazoline and thiazine with dibro- mides and their structures were characterized by IR, 1H NMR, MS and elemental analysis. The synthesized derivatives were tested for antitumor activity.展开更多
1,2-O-Isopropylidene-5-O-p-toluenesulfonyl-α-D-erythro-pentofuranos-3-ulose 1 was treated with thiourea and aminothiourea to give a D-ribose derivative 2 bearing a 2-amino 1,3-thiazine ring and a thiosemicarbazone de...1,2-O-Isopropylidene-5-O-p-toluenesulfonyl-α-D-erythro-pentofuranos-3-ulose 1 was treated with thiourea and aminothiourea to give a D-ribose derivative 2 bearing a 2-amino 1,3-thiazine ring and a thiosemicarbazone derivative 5, respectively. 2 was acylated with Ac20 and propandioic acid to afford two acylation derivatives 3 and 4, respectively. Reduction of 5 with NaBH4 in methanol produced a hydrothiosemicarbazone derivative 6. The absolute configuration of 2 was confirmed by X-ray crystallographic analysis. The structures of all products were elucidated by IR, NMR and HRMS spectra.展开更多
Methylene blue(MB) is commonly used in aquaculture as a fungicide and antidotes. This study was designed to explore the pharmacokinetics of MB in Japanese eel(Anguilla Japonica) immersed in 10 mg L^-1 and 20 mg L^-1 M...Methylene blue(MB) is commonly used in aquaculture as a fungicide and antidotes. This study was designed to explore the pharmacokinetics of MB in Japanese eel(Anguilla Japonica) immersed in 10 mg L^-1 and 20 mg L^-1 MB for 0.5 h. The concentrations of MB and its derivatives in the blood, liver, kidney, skin and muscle were determined by HPLC after immersion. The results showed that the changes of drug concentrations in Japanese eel were basically the same in different dose groups, showing a general trend of increasing at first and then decreasing, but the peak time was slightly different. The peak concentration of the drug was positively correlated with the dose level. The peak concentrations of MB in MB(20 mg L^-1) group, MB, azure A and azure B in the tissues of Japanese eel were significantly higher than those in MB(10 mg L^-1) group. Moreover, MB, azure A and azure B remained for a long time and could still be detected at 64 days, and azure C was not detected in tissues.展开更多
A practical method for the construction of difluoromethylene-containing 1,4-thiazine moieties using readily available diethyl bromodifluoromethanephosphonate(BrCF_(2)PO(OEt)_(2))as difluorocarbene precusor has been de...A practical method for the construction of difluoromethylene-containing 1,4-thiazine moieties using readily available diethyl bromodifluoromethanephosphonate(BrCF_(2)PO(OEt)_(2))as difluorocarbene precusor has been developed.This transformation features the efficient capture of difluorocarbene by pyridinium 1,4-zwitterionic thiolates.A series of structurally novel and functionalized difluoromethylene-containing 1,4-thiazine derivatives were thus synthesized in good yields.展开更多
The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferre...The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferred into cytotoxic triazoles by alkylation and ＂click＂ synthesis in satisfactory yields of 87%^95%. Their structures were characterized by IR, H-RESI-MS and NMR analysis. Meanwhile, the crystal of Ⅲ was obtained and determined by X-ray single-crystal diffraction. Crystal data： orthorhombic system, space group P212121, a = 5.189（4）, b = 8.661（6）, c = 23.498（17） A, V = 1056.2（13） A^3, Z = 4, F（000） = 464, Dc = 1.392 g/cm^3, μ =0.284 mm^-1, R = 0.0637 and wR = 0.1668 for 8182 independent reflections（R（int） = 0.1580） and 2166 observed ones（I 〉 2σ（I））.展开更多
Unprecedented cycloaddition reactions of azatrienes (1) with sulfene leading to the synthesis of functionalized thiazinedioxide derivatives (5) are described. The reactions were found be highly regioselective resultin...Unprecedented cycloaddition reactions of azatrienes (1) with sulfene leading to the synthesis of functionalized thiazinedioxide derivatives (5) are described. The reactions were found be highly regioselective resulting in the formation of only [4 + 2] cycloadducts.展开更多
文摘Thiazine sugar derivative 2 was synthesized and characterized by IR, NMR and H RMS, and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system （C16H24N2O8S2, Mr = 436.49） with space group P21, a = 10.311（2）, b = 9.1198（18）, c = 11.623（2）A, β = 109.47（3）°, V= 1030.4（4）A^3, Z= 2, Dc = 1.407 g/cm^3, F（000）= 460, μ= 0.303 mm^-1, the final R = 0.0437 and wR = 0.0561 for 1954 observed reflections （I 〉 2σ（I））. Nine hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparison with the original material.
文摘A series of novel multithioether derivatives were synthesized by the combination of thiazoline and thiazine with dibro- mides and their structures were characterized by IR, 1H NMR, MS and elemental analysis. The synthesized derivatives were tested for antitumor activity.
基金the National Natural Science Foundation of China(No.20472075)for financial support of this work.
文摘1,2-O-Isopropylidene-5-O-p-toluenesulfonyl-α-D-erythro-pentofuranos-3-ulose 1 was treated with thiourea and aminothiourea to give a D-ribose derivative 2 bearing a 2-amino 1,3-thiazine ring and a thiosemicarbazone derivative 5, respectively. 2 was acylated with Ac20 and propandioic acid to afford two acylation derivatives 3 and 4, respectively. Reduction of 5 with NaBH4 in methanol produced a hydrothiosemicarbazone derivative 6. The absolute configuration of 2 was confirmed by X-ray crystallographic analysis. The structures of all products were elucidated by IR, NMR and HRMS spectra.
基金supported by the National Key R&D Program of China (No.2019YFD0900102)the Science and Technology Commission of Shanghai Municipality (Nos.17050502100 and 18391901500)+1 种基金the National Natural Resources Platform of ChinaKnowledge Service Platform of Shanghai Ocean University。
文摘Methylene blue(MB) is commonly used in aquaculture as a fungicide and antidotes. This study was designed to explore the pharmacokinetics of MB in Japanese eel(Anguilla Japonica) immersed in 10 mg L^-1 and 20 mg L^-1 MB for 0.5 h. The concentrations of MB and its derivatives in the blood, liver, kidney, skin and muscle were determined by HPLC after immersion. The results showed that the changes of drug concentrations in Japanese eel were basically the same in different dose groups, showing a general trend of increasing at first and then decreasing, but the peak time was slightly different. The peak concentration of the drug was positively correlated with the dose level. The peak concentrations of MB in MB(20 mg L^-1) group, MB, azure A and azure B in the tissues of Japanese eel were significantly higher than those in MB(10 mg L^-1) group. Moreover, MB, azure A and azure B remained for a long time and could still be detected at 64 days, and azure C was not detected in tissues.
基金Financial support from National Natural Science Foundation of China(Nos.21931013 and 22271105)Natural Science Foundation of Fujian Province(No.2022J02009)+2 种基金Open Research Fund of School of Chemistry and Chemical Engineering,Henan Normal Universitythe Instrumental Analysis Center of Huaqiao University for analysis supportthe Subsidized Project for Cultivating Postgraduates’Innovative Ability in Scientific Research of Huaqiao University。
文摘A practical method for the construction of difluoromethylene-containing 1,4-thiazine moieties using readily available diethyl bromodifluoromethanephosphonate(BrCF_(2)PO(OEt)_(2))as difluorocarbene precusor has been developed.This transformation features the efficient capture of difluorocarbene by pyridinium 1,4-zwitterionic thiolates.A series of structurally novel and functionalized difluoromethylene-containing 1,4-thiazine derivatives were thus synthesized in good yields.
基金Supported by the National Natural Science Foundation of China(No.21272136)Scientific Foundation from graduate school(2015CX131)Youth Talent Development Foundation of China Three Gorges University
文摘The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferred into cytotoxic triazoles by alkylation and ＂click＂ synthesis in satisfactory yields of 87%^95%. Their structures were characterized by IR, H-RESI-MS and NMR analysis. Meanwhile, the crystal of Ⅲ was obtained and determined by X-ray single-crystal diffraction. Crystal data： orthorhombic system, space group P212121, a = 5.189（4）, b = 8.661（6）, c = 23.498（17） A, V = 1056.2（13） A^3, Z = 4, F（000） = 464, Dc = 1.392 g/cm^3, μ =0.284 mm^-1, R = 0.0637 and wR = 0.1668 for 8182 independent reflections（R（int） = 0.1580） and 2166 observed ones（I 〉 2σ（I））.
文摘Unprecedented cycloaddition reactions of azatrienes (1) with sulfene leading to the synthesis of functionalized thiazinedioxide derivatives (5) are described. The reactions were found be highly regioselective resulting in the formation of only [4 + 2] cycloadducts.
