A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux cond...A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux conditions. 3,12-dimethylbenzo[a]quinoxalino[2,3-c] phenazine with bidentate character reacts with mercury（II） bromide to give suitable crystals. All products were confirmed by IR, ^1H and ^13C NMR, and the metal complex by single-crystal X-ray method. The crystal（C24H16Br2HgN4, Mr = 720.82） belongs to the triclinic system, space group P1 with a = 10.186（6）, b = 10.421（6）, c = 11.470（7） A, α = 98.670（7）, β = 95.069（7）, γ = 109.831（7）°, V = 1119.4（12） A3, Z = 2, Dc = 2.139 Mg/m^3, μ = 10.46 mm^-1, F（000） = 676, R = 0.043 and wR = 0.115 for 3982 observed reflections with I 〉 2σ（I）.展开更多
通过添加抗氧化剂四氢呋喃和抗坏血酸,对传统的二硫代氨基甲酸酯类化合物检测方法——1,2-苯二硫酚衍生-高效液相色谱法进行了优化和改进,并用4种常用二硫代氨基甲酸酯类杀菌剂[70%代森锰锌可湿性粉剂(WP)、68%精甲霜锰锌水分散粒剂(WG)...通过添加抗氧化剂四氢呋喃和抗坏血酸,对传统的二硫代氨基甲酸酯类化合物检测方法——1,2-苯二硫酚衍生-高效液相色谱法进行了优化和改进,并用4种常用二硫代氨基甲酸酯类杀菌剂[70%代森锰锌可湿性粉剂(WP)、68%精甲霜锰锌水分散粒剂(WG)、68%霜脲锰锌WG和55%唑醚代森联WG]对该方法进行了验证。结果表明:当1,2-苯二硫酚浓度为12 mmol/L、代森锰锌用乙二胺四乙酸二钠(EDTA,p H 9.3)及代森联用二乙基三胺五乙酸(DTPA,p H 10.0)解络合、且同时添加体积分数为4%的四氢呋喃和40 mg/L的抗坏血酸时衍生化条件最优。除55%唑醚代森联WG外,其他3种商品杀菌剂待测液在衍生化后48 h内均保持稳定且相对标准偏差<5%,满足测试要求。该方法操作简便快捷,检出目标物明确,不受二硫代氨基甲酸酯类杀菌剂常见代谢物乙撑硫脲及二硫化碳的影响,检测效率高,适用于该类杀菌剂的批量测试。展开更多
Keggin type heteropolyacids was found to be an efficient and reusable catalyst for the synthesis of biologically active quinoxaline derivatives from the condensation of 1,2-diamine with 1,2-dicarbonyl compounds in exc...Keggin type heteropolyacids was found to be an efficient and reusable catalyst for the synthesis of biologically active quinoxaline derivatives from the condensation of 1,2-diamine with 1,2-dicarbonyl compounds in excellent yields in water. This method provides a new and efficient protocol in terms of small quantity of catalyst, a wide scope of substrates, and simple work-up procedure.展开更多
The title compound C18H16N4O3 （Mr = 336.35） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect...The title compound C18H16N4O3 （Mr = 336.35） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632（1）, b = 7.816（1）, c = 28.082（5） A,β = 96.18（1）°, V= 1665.48（51） A^3, Z= 4, Dc = 1.341 g/cm^3, F（000） = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C（11）-C（16） phenyl ring, which are approximately coplanar （r.m.s. de deviation from the combined mean plane is 0.03 A） with the dihedral angle between them of 9.8%.展开更多
The title compound （C16H15N3O2, Mr= 281.31） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect...The title compound （C16H15N3O2, Mr= 281.31） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150（3）, b = 9.906（3）, c = 13.624（4） A, β = 106.360（4）°, V= 1443.9（7） ,A^3, Z = 4, Dc = 1.294 g/cm^3, F（000） = 592,μ（MoKa） = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O（2）-C（10） phenyl ring, which are approximately coplanar （r.m.s. de deviation from the combined mean plane is 0026 A） with the dihedral angle between them of 6.3°.展开更多
文摘A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux conditions. 3,12-dimethylbenzo[a]quinoxalino[2,3-c] phenazine with bidentate character reacts with mercury（II） bromide to give suitable crystals. All products were confirmed by IR, ^1H and ^13C NMR, and the metal complex by single-crystal X-ray method. The crystal（C24H16Br2HgN4, Mr = 720.82） belongs to the triclinic system, space group P1 with a = 10.186（6）, b = 10.421（6）, c = 11.470（7） A, α = 98.670（7）, β = 95.069（7）, γ = 109.831（7）°, V = 1119.4（12） A3, Z = 2, Dc = 2.139 Mg/m^3, μ = 10.46 mm^-1, F（000） = 676, R = 0.043 and wR = 0.115 for 3982 observed reflections with I 〉 2σ（I）.
文摘通过添加抗氧化剂四氢呋喃和抗坏血酸,对传统的二硫代氨基甲酸酯类化合物检测方法——1,2-苯二硫酚衍生-高效液相色谱法进行了优化和改进,并用4种常用二硫代氨基甲酸酯类杀菌剂[70%代森锰锌可湿性粉剂(WP)、68%精甲霜锰锌水分散粒剂(WG)、68%霜脲锰锌WG和55%唑醚代森联WG]对该方法进行了验证。结果表明:当1,2-苯二硫酚浓度为12 mmol/L、代森锰锌用乙二胺四乙酸二钠(EDTA,p H 9.3)及代森联用二乙基三胺五乙酸(DTPA,p H 10.0)解络合、且同时添加体积分数为4%的四氢呋喃和40 mg/L的抗坏血酸时衍生化条件最优。除55%唑醚代森联WG外,其他3种商品杀菌剂待测液在衍生化后48 h内均保持稳定且相对标准偏差<5%,满足测试要求。该方法操作简便快捷,检出目标物明确,不受二硫代氨基甲酸酯类杀菌剂常见代谢物乙撑硫脲及二硫化碳的影响,检测效率高,适用于该类杀菌剂的批量测试。
基金supported by the Ministry of Science and Technology of China (2014CB239402, 2017YFA0206903)the National Natural Science foundation of China (21390404)+1 种基金the Strategic Priority Research Program of the Chinese Academy of Science (XDB17000000)the Key Research Pro-gram of Frontier Sciences, the Chinese Academy of Sciences (QYZDY-SSW-JSC029)~~
文摘Keggin type heteropolyacids was found to be an efficient and reusable catalyst for the synthesis of biologically active quinoxaline derivatives from the condensation of 1,2-diamine with 1,2-dicarbonyl compounds in excellent yields in water. This method provides a new and efficient protocol in terms of small quantity of catalyst, a wide scope of substrates, and simple work-up procedure.
文摘The title compound C18H16N4O3 （Mr = 336.35） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632（1）, b = 7.816（1）, c = 28.082（5） A,β = 96.18（1）°, V= 1665.48（51） A^3, Z= 4, Dc = 1.341 g/cm^3, F（000） = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C（11）-C（16） phenyl ring, which are approximately coplanar （r.m.s. de deviation from the combined mean plane is 0.03 A） with the dihedral angle between them of 9.8%.
基金This work was supported by the Phytochemistry Key Laboratory of Shaanxi Province (No. 02js40)
文摘The title compound （C16H15N3O2, Mr= 281.31） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150（3）, b = 9.906（3）, c = 13.624（4） A, β = 106.360（4）°, V= 1443.9（7） ,A^3, Z = 4, Dc = 1.294 g/cm^3, F（000） = 592,μ（MoKa） = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O（2）-C（10） phenyl ring, which are approximately coplanar （r.m.s. de deviation from the combined mean plane is 0026 A） with the dihedral angle between them of 6.3°.
