A new coordination polymer, namely [Zn（pdc）（bbi）]n {H2 pdc = 2,3-pyridine dicar- boxylic acid, bbi = 1,1-（1,4-butanediyl）bis（imidazole）}, has been prepared under hydrothermal conditions and characterized by el...A new coordination polymer, namely [Zn（pdc）（bbi）]n {H2 pdc = 2,3-pyridine dicar- boxylic acid, bbi = 1,1-（1,4-butanediyl）bis（imidazole）}, has been prepared under hydrothermal conditions and characterized by elemental analysis, IR, and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21 /n with a = 8.436（3）, b = 16.988（5）, c = 12.106（4）, β = 92.204（5）°, V = 1733.6（9）3, Z = 4, C17 H17 N5 O4 Zn, Mr = 420.73, Dc = 1.612 g/cm3, F（000） = 864, μ（MoKa） = 0.452 mm-1, the R = 0.0672 and wR = 0.1645. In the mononuclear complex, each Zn（II） is five-coordinated by one carboxylate O and one pyridyl N atoms from one pdc anion, one carboxylate O atom from another pdc anion, and two N atoms from two bib ligands. The Zn（II） ions are connected by pdc ligands to form skeleton chains, and bbi ligands further link them to construct a 2D framework. The thermal and luminescence properties of the complex were also investigated.展开更多
2,3-Dichlorobenzoic acid was prepared from 2,3-dichloroaniline by diazotization and Sandmeyerreaction to give 2,3-dichlorobenzonitrile and followed by hydrolysis with an overall yield of 58%.
New highly stereoregular 2, 3 -di- O-(p-azidobenzyl )-(1 →5 ) - α-D -ribofuranan was synthesized byselective ring-opening polymerization of 1, 4-anhydro-2, 3 - di-O -(p-azidobenzyl )-α-D -ribopyranose(ADABR) using ...New highly stereoregular 2, 3 -di- O-(p-azidobenzyl )-(1 →5 ) - α-D -ribofuranan was synthesized byselective ring-opening polymerization of 1, 4-anhydro-2, 3 - di-O -(p-azidobenzyl )-α-D -ribopyranose(ADABR) using phosphorus pentafluoride or tin tetrachloride as catalyst at low temperature indichloromethane. The monomer was obtained by the reaction of p - bromomethyl -phenyleneazide with 1, 4 -anhydro-α-D-ribose in DMF. The structure of poly(ADANR) was identified by specific rotation and ^(13)C-NMR spectroscopy. Acid chloride-AgCl_4 complex catalyst such as CH_2=C(CH_3)C^+OClO_4^- used in thepolymerization resulted in polymers with mixed structures, i.e. (1→5)-α-D-ribofuranosidic and (1→4)-β-D-ribopyranosidic units. However, with C_6H_5C^+OClO_4^- as catalyst, pure (1→5)-α-D-ribofuranan was obtained.The effects of catalyst, polymerization temperature and time on polymer stereoregularity were examined, andthe mechanism of the ring-opening polymerization was discussed.展开更多
The chiral compound 5H-imidazol[2,3-b]isoquinoline-l-ethanol-5-one-1,2, 3, 10b-tetrahydro- β（S）-phenyl-3（S）-phenyl was synthesized from the direct condensation of 2- cyanophenyacetonitrile with optically active ...The chiral compound 5H-imidazol[2,3-b]isoquinoline-l-ethanol-5-one-1,2, 3, 10b-tetrahydro- β（S）-phenyl-3（S）-phenyl was synthesized from the direct condensation of 2- cyanophenyacetonitrile with optically active （S）-（＋）-2-phenylglycinol in chlorobenzene under dry, anaerobic conditions. ZnCl2 was used as a Lewis acid catalyst in this reaction, and the structure of this compound was determined by X-ray diffraction, NMR, MS and IR. Crystal data of the title compound： C25H22N2O2, Mr = 382.45, P 21 21 21, a = 5.341（5）, b = 16.735（5）, c = 22.129（5） A, γ = 90°, V = 1978（2）A^3, Z = 4, Dc = 1.284 g/cm^3, the final R = 0.0321 for 2269 observed reflections with I 〉 2 σ（I） and Rw = 0.0771 for all data.展开更多
目的:建立拉莫三嗪原料药有关物质的HPLC测定方法。方法:采用Feini Gen Red ClassicalⅡC18(250 mm×4.6 mm,5μm)色谱柱,对拉莫三嗪的有关物质进行定量分析,以磷酸二氢钾缓冲液(取磷酸二氢钾2.7 g,加水800 m L使溶解,加三乙胺6.7 m...目的:建立拉莫三嗪原料药有关物质的HPLC测定方法。方法:采用Feini Gen Red ClassicalⅡC18(250 mm×4.6 mm,5μm)色谱柱,对拉莫三嗪的有关物质进行定量分析,以磷酸二氢钾缓冲液(取磷酸二氢钾2.7 g,加水800 m L使溶解,加三乙胺6.7 m L,用磷酸调节p H至2.0,加水至1 000 m L)为流动相A,乙腈为流动相B,梯度洗脱,流速为1.5 m L·min-1,柱温为35℃,检测波长为210 nm(用于检测2,3-二氯苯甲酸)和270 nm(用于检测除2,3-二氯苯甲酸外的其他杂质)。用HPLC-MS鉴定氧化降解溶液中未知杂质;采用Thermo AcclaimTM120 C18(250 mm×4.6 mm,5μm)色谱柱,以甲醇-水(50∶50)为流动相,ESI离子源,正离子扫描方式,检测离子m/z为272。结果:主峰与各有关物质峰分离度良好,拉莫三嗪及各有关物质在质量浓度为0.3~4.0μg·m L-1范围内呈良好的线性关系(r2=0.998 7),拉莫三嗪的定量下限为0.2μg·m L-1(270 nm)、杂质Ⅰ的定量下限为0.2μg·m L-1(210 nm)。3批样品有关物质测定结果显示,已知杂质和未知杂质均未检出。结论:本法可为拉莫三嗪质量控制提供参考。展开更多
基金Supported by the Key Scientific and Technological Project of Henan(122102210250)the Foundation of Henan Educational Committee(13A150102)the key disciplines of analytical chemistry of Henan province
文摘A new coordination polymer, namely [Zn（pdc）（bbi）]n {H2 pdc = 2,3-pyridine dicar- boxylic acid, bbi = 1,1-（1,4-butanediyl）bis（imidazole）}, has been prepared under hydrothermal conditions and characterized by elemental analysis, IR, and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21 /n with a = 8.436（3）, b = 16.988（5）, c = 12.106（4）, β = 92.204（5）°, V = 1733.6（9）3, Z = 4, C17 H17 N5 O4 Zn, Mr = 420.73, Dc = 1.612 g/cm3, F（000） = 864, μ（MoKa） = 0.452 mm-1, the R = 0.0672 and wR = 0.1645. In the mononuclear complex, each Zn（II） is five-coordinated by one carboxylate O and one pyridyl N atoms from one pdc anion, one carboxylate O atom from another pdc anion, and two N atoms from two bib ligands. The Zn（II） ions are connected by pdc ligands to form skeleton chains, and bbi ligands further link them to construct a 2D framework. The thermal and luminescence properties of the complex were also investigated.
文摘2,3-Dichlorobenzoic acid was prepared from 2,3-dichloroaniline by diazotization and Sandmeyerreaction to give 2,3-dichlorobenzonitrile and followed by hydrolysis with an overall yield of 58%.
文摘New highly stereoregular 2, 3 -di- O-(p-azidobenzyl )-(1 →5 ) - α-D -ribofuranan was synthesized byselective ring-opening polymerization of 1, 4-anhydro-2, 3 - di-O -(p-azidobenzyl )-α-D -ribopyranose(ADABR) using phosphorus pentafluoride or tin tetrachloride as catalyst at low temperature indichloromethane. The monomer was obtained by the reaction of p - bromomethyl -phenyleneazide with 1, 4 -anhydro-α-D-ribose in DMF. The structure of poly(ADANR) was identified by specific rotation and ^(13)C-NMR spectroscopy. Acid chloride-AgCl_4 complex catalyst such as CH_2=C(CH_3)C^+OClO_4^- used in thepolymerization resulted in polymers with mixed structures, i.e. (1→5)-α-D-ribofuranosidic and (1→4)-β-D-ribopyranosidic units. However, with C_6H_5C^+OClO_4^- as catalyst, pure (1→5)-α-D-ribofuranan was obtained.The effects of catalyst, polymerization temperature and time on polymer stereoregularity were examined, andthe mechanism of the ring-opening polymerization was discussed.
文摘The chiral compound 5H-imidazol[2,3-b]isoquinoline-l-ethanol-5-one-1,2, 3, 10b-tetrahydro- β（S）-phenyl-3（S）-phenyl was synthesized from the direct condensation of 2- cyanophenyacetonitrile with optically active （S）-（＋）-2-phenylglycinol in chlorobenzene under dry, anaerobic conditions. ZnCl2 was used as a Lewis acid catalyst in this reaction, and the structure of this compound was determined by X-ray diffraction, NMR, MS and IR. Crystal data of the title compound： C25H22N2O2, Mr = 382.45, P 21 21 21, a = 5.341（5）, b = 16.735（5）, c = 22.129（5） A, γ = 90°, V = 1978（2）A^3, Z = 4, Dc = 1.284 g/cm^3, the final R = 0.0321 for 2269 observed reflections with I 〉 2 σ（I） and Rw = 0.0771 for all data.
文摘目的:建立拉莫三嗪原料药有关物质的HPLC测定方法。方法:采用Feini Gen Red ClassicalⅡC18(250 mm×4.6 mm,5μm)色谱柱,对拉莫三嗪的有关物质进行定量分析,以磷酸二氢钾缓冲液(取磷酸二氢钾2.7 g,加水800 m L使溶解,加三乙胺6.7 m L,用磷酸调节p H至2.0,加水至1 000 m L)为流动相A,乙腈为流动相B,梯度洗脱,流速为1.5 m L·min-1,柱温为35℃,检测波长为210 nm(用于检测2,3-二氯苯甲酸)和270 nm(用于检测除2,3-二氯苯甲酸外的其他杂质)。用HPLC-MS鉴定氧化降解溶液中未知杂质;采用Thermo AcclaimTM120 C18(250 mm×4.6 mm,5μm)色谱柱,以甲醇-水(50∶50)为流动相,ESI离子源,正离子扫描方式,检测离子m/z为272。结果:主峰与各有关物质峰分离度良好,拉莫三嗪及各有关物质在质量浓度为0.3~4.0μg·m L-1范围内呈良好的线性关系(r2=0.998 7),拉莫三嗪的定量下限为0.2μg·m L-1(270 nm)、杂质Ⅰ的定量下限为0.2μg·m L-1(210 nm)。3批样品有关物质测定结果显示,已知杂质和未知杂质均未检出。结论:本法可为拉莫三嗪质量控制提供参考。
