catena‐Poly[[[pyridinecopper(II)]bis[μ3‐4‐(2‐oxidobenzylideneamino)benzoato]] dimethylformamide disolvate], a polymer composed of dimeric dicopper building units

The title compound, {[Cu(C₁₄H₉NO₃)(C₅H₅N)]·C₃H₇NO}_n or {[Cu₂L₂(py)₂]·2DMF}_n [py is pyridine, L is 4‐(salicylideneamino)benzoate and DMF is dimethylformamide], is composed of dimeric dicopper [CuL(py)]₂ building units, which are interlinked into a one‐dimensional chain through the formation of Cu—O_COO bonds. The dimeric unit is centrosymmetric, containing two Cu^II atoms linked by bridging phenolate O atoms into a Cu₂O₂ plane with a chelating Cu—O bond length of 1.927 (2) Å and a bridging Cu—O bond length of 2.440 (2) Å. Interchain C—H...O and π–π stacking interactions are responsible for an extensive three‐dimensional structure in which the resulting channels are filled by DMF solvent molecules.     

Syntheses and Crystal Structures of Cadmium Complexes with Thiophenedicarboxylate and Bipyridine‐like Ligands

Two new coordination polymers [Cd(tdc)(bpy)(H₂O)]_n ( 1 ) and [Cd(tdc)(phen)]_n ( 2 ) (H₂tdc = thiophene‐2,5‐dicarboxylic acid, bpy = 2,2′‐bipyridine and phen = 1,10‐phenanthroline) have been synthesized under hydrothermal condition. Their crystal structures have been established by X‐ray single‐crystal diffraction. Complex 1 crystallizes in the orthorhombic space group Fdd2 with a = 14.757(7), b = 45.38(2), c = 10.518(5) Å, V = 7044(6) ų, Z = 16; 2 in the monoclinic space group P2₁/c with a = 7.262(1), b = 21.970(2), c = 10.051(1) Å, β = 105.01(1)°, V = 1548.8(2) ų, Z = 4. Both of them are double‐stranded chains and further assembled into three‐dimensional networks by π‐π stacking interactions. 1 and 2 are stable in air, and show blue photoluminescence at 415 nm and 410 nm, respectively.     

诱导效应指数与脂肪族胺、醇和醚的气相碱性

用烷基诱导效应指数I和RX分子中质子亲合原子X所带电荷qx及元素电负性XN与 脂肪胺，醇、醚的气相质子亲合PA进行关联，结果表明，脂肪胺，醇、醚的气相碱 性可以用下式定量描述：PA(kJ.mol^-1)-2732.0333-2457.1510∑I-1492.2351qx- 732.6277XN利用上式对64种化合物的气相碱性进行预测，平均相对误差为0．34％ ，预测值和实验值的偏差均在实验误差范围内。     

甲状腺机能亢进症头发锌、硒、钒、锂、锗5种微量元素的动态变化

测定了２４例甲亢治疗前后及３０例健康对照的头发锌、硒、钒、锂及锗的含量，发现未治疗的甲亢头发锌、硒、钒、锂及锗含量较对照组低，Ｚｎ、Ｓｅ、Ｌｉ、Ｇｅ，Ｐ＜０．００１，Ｖ，Ｐ＜０．０１．甲亢经６～１２周抗甲亢药物治疗后．头发中５种元素均较治疗前上升（Ｐ＜０．００１），且头发钒和锂含量治疗后已达到对照组水平，Ｖ，Ｐ＞０．２，Ｌｉ，Ｐ＞０．１，而头发锌、晒及锗含量治疗后仍低于对照组（Ｐ＜０　．００１）．结论：甲亢头发锌、硒、钒、锂及锗含量降低．经６～１２周抗甲亢治疗可使头发钒及锂含量恢复正常水平，而其余３种元素则可能需要更长时间的抗甲亢治疗才能恢复至正常水平。     

Highly stereoselective three-component reactions of phenylselenomagnesium bromide,acetylenic sulfones,and saturated aldehydes/ketones or alpha,beta-unsaturated enals or enones

beta-Phenylseleno-alpha-tolylsulfonyl-substituted alkenes were synthesized via the three-component conjugate-nucleophilic addition of acetylenic sulfones, phenylselenomagnesium bromide, and carbonyl compounds, such as aldehydes, aliphatic ketones, or alpha,beta-unsaturated enals or enones. The reaction is highly regio- and stereoselective with moderate to good yields. Functionalized allylic alcohols were obtained in the case of aldehydes and aliphatic ketones. In the case of alpha,beta-unsaturated enones, functionalized allylic alcohols or functionalized gamma,delta-unsaturated ketones were obtained, depending on the structures of the ketones.     

新型四硫代富瓦烯衍生物的合成及其性质的研究

合成了3个新的含有卤素取代基的四硫代富瓦烯衍生物及6个新的相关化合物。利用溶液的电子吸收光谱对四硫代富瓦烯衍生物的性质进行了研究。研究结果表明, 四硫代富瓦烯衍生物的分子中π轨道之间的能级差较小, 因而分子具有较高的稳定性。     

磁载纳米TiO2光催化剂的制备及其光催化性能研究

采用肼((NH2)2*H2O)还原硝酸铁(Fe(NO3)3)法制备纳米级磁基体(Fe3O4), 以聚乙二醇对其表面进行改性, 通过溶胶-凝胶法制得TiO2/Fe3O4磁载纳米TiO2光催化剂, 并用于光催化降解橙黄-II, 对其活性进行评价. 结果表明 TiO2/Fe3O4光催化剂的降解率在第一次使用时与纯TiO2相近, 三次循环使用后, 仍能保持较高的催化活性. 催化剂的最佳用量为4 g/L, 在酸性和碱性环境中均能保持很好的催化活性.     

室温离子液体EMIES的标准生成焓

在(298.15 ±0.01) K下用转动弹热量计测定了离子液体硫酸乙酯-1-甲基-3-乙基咪唑(EMIES)及合成它的原料1-甲基咪唑的恒容燃烧热,通过计算得到它们的标准燃烧焓 分别为(－2671±2) 和(－286.3±0.5) kJ·mol－1;标准生成焓 分别为(－3060±3) kJ·mol－1和(－2145±4) kJ·mol－1.结合文献上硫酸二乙酯的标准生成焓数据,得到了合成离子液体EMIES的反应热(－102.3±1.0) kJ·mol－1,与合成实验中观察到的强烈放热现象是一致的.根据离子液体EMIES的热容数据,计算了不同温度下EMIES的标准生成焓.     

指纹图谱法在参麦注射液质控中的应用

 中医药理论和实践要求综合评价中药的质量 ,指纹图谱法是对中药制剂进行综合宏观分析的可行手段之一 ,因此采用反相高效液相建立了参麦注射液的特征指纹图谱。条件 :Hypersil C18(4 6mmi d × 2 5 0mm ,5 μm)反相柱 ,流动相由水 (A)和乙腈 (B)组成 ,B的体积分数在 5 0min内由 5 %线性增长到 95 % ,流速为1 0mL/min ;紫外检测 ,波长为 2 0 2nm。 2 3个特征指纹峰与内标 (联苯 )的峰面积比作为指标 ,结合主成分分析 投影判别法比较了同一厂家不同批次产品和不同厂家同类产品的化学指纹差异。     

Solid-phase Synthesis of-Haloaldehydes from Polymer-supported 4-(Phenylseleno)morpholine

Polymer-supported reagents for organic synthesis are enjoying a renewed popularity with the emergence of combinatorial chemistry in recent years1. 4-(Arylseleno)morpholines formed in situ are useful -seleno-introducing reagents for saturated aldehydes2. -Sele- noaldehydes, as a frequently used intermediates, can be converted into -haloaldehydes by halogenating reaction3. However, organic selenium reagents always have a foul smell and are quite toxic, which is often problematic in organic sy…