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251.
建立了分离测定萘普生和溴代萘普生的反相键合相高效液相色谱法。采用ODS柱,以添加50mmol/L乳酸并用高氯酸调节pH为2.5的80%甲醇-水溶液作为流动相,以苯甲酸为内标物,测定了不对称合成工艺产物中萘普生和溴代萘普生的含量。方法的准确度分别为99.83%~102.07%(萘普生)和99.0%~100.83%(溴代萘普生),相对标准偏差分别小于2.58%(萘普生)和3.64%(溴代萘普生)。方法可用于工艺条件的选择和质量检测。 相似文献
252.
253.
18-冠-6与Eu(fod)3+在CCl4中的化学平衡及其配合物的结构 总被引:1,自引:0,他引:1
在室温下测定了CCl_4溶液中,18-冠-6的亚甲基、Eu(fod)的t—丁基质子的PMR化学位移与溶液组成的相互关系。提出了生成配合物RS,R_2S,R_2,R_3(S为18-冠-6,R为Eu(fod)_3)的模式。求得了平衡常数值(升/摩):K_1=[RS]/([R][S])=2.O×10~5,K_2=[R_2S]/([R][RS])=1.0×10~3,Q_1=[R_2]/[R]~2=4.2×10~2,Q_2=[R_3]/([R_2][R])=4.0×10~1。并测得在配合物RS,R_2S中18-冠-6质子的平均化学位移分别为4.90,10.84(ppm,相对于纯18-冠-6); 在配合物R,R_2,R_3,RS,R_2中t-丁基质子平均化学位移分别为1.53,2.33,0.54,1.02,2.42(ppm,相对于TMS)。 根据配合物的化学位移值,并考虑分子及分子轨道的对称性、位阻等因素提出了配合物R_2,RS,R_2S的可能的结构模型。 相似文献
254.
微量元素锌与反复呼吸道感染的相关性 总被引:2,自引:1,他引:2
陈洁 《广东微量元素科学》1996,3(1):22-23
对28例反复呼吸道感染患儿(下称复感儿)及26例健康儿进行微量元素发锌测定。发现前者发锌平均值为(92.3±14.7)×10~(-6),后者为(132.5±21.5)×10~(-6),P<0.01,差异非常显著。对复感儿进行口服锌治疗,观察其疗效及治疗前后发锌变化。治疗前发锌平均值为(92.3±14.7)×10~(-6),治疗后为(137.5±20.2)×10~(-6),P<0.01差异非常显著。有效率达85.7%。故缺锌可能是复感儿患病的影响因素之一,锌治疗小儿反复呼吸道感染是十分必要的。 相似文献
255.
Liya?Wang Zhiliang?Liu Chenxi?Zhang Zhanquan?Liu Daizheng?Liao Zonghui?JiangEmail author Shiping?Yan 《中国科学B辑(英文版)》2003,46(6):533-541
A novel one-dimensional manganese(II) complex containing nitronyl nitroxide radical [Mn2(IM2-py)2(Ac)2(μ1,1-N3)(μ1,3-N3) · EtOH]
n
was synthesized and characterized structurally and magnetically. It crystallizes in the monoclinic space group p21/n. Each Mn(II) ion is six-coordinated in a distorted octahedral environment. The two N atoms of the nitronyl nitroxide radical
and the two O atoms of acetate ligands are in the equatorial plane, whereas the two different azido bridging ligands are in
trans axial position. Mn(II) ions are linked by nitrogen atom of μ1,1-azido and oxygen atoms of two carboxy groups to form a Mn-Mn unit. Mn-Mn units are linked by azido ligands through μ1,3 bridging style to form a one-dimensional chain. The compound is connected by the coordination bonds, π-π interactions and
hydrogen bonds as a three-dimensional structure. Magnetic susceptibility data support that there are stronger antiferromagnetic
interactions between the radical and Mn(II) ion, weak antiferromagnetic interactions between the Mn-R units, and very weak
antiferromagnetic interactions between the R-Mn-Mn-R units. 相似文献
256.
A novel carrier of ultradispersed diamond black powder (UDDBP) was used to support metallocene catalyst. Al2O3 was also used as carrier in order to compare with UDDBP. Supported catalysts for ethylene polymerization were synthesized by two different reaction methods. One way was direct immobilization of the metallocene on the support, the other was adsorption of MAO onto the support followed by addition of the metallocene. Four supported catalysts Cp2ZrCl2/UDDBP, Cp2ZrCl2/Al2O3, Cp2ZrCl2/MAO/UDDBP and Cp2ZrCl2/Al2O3/MAO were obtained. The content of the zirconium in the supported catalyst was determined by UV spectroscopy. The activity of the ethylene polymerization catalyzed by supported catalyst was investigated. The influence of Al/Zr molar ratio and polymerization temperature on the activity was discussed. The polymerization rate was also observed. 相似文献
257.
《Tetrahedron: Asymmetry》2006,17(6):900-907
Recently prepared chiral amines have been used in the preparation of novel tridentate ligands based on an imidazole ring with an additional (hetero)ring. The synthesis was carried out by the reaction of chiral amines with suitable aldehydes (2-phenylimidazole-4-carbaldehyde, 2-hydroxybenzaldehyde or pyridine-2-carbaldehyde) under reductive conditions (H2/Pd or NaBH4). All ligands prepared showed strong hydrogen bonds in d6-DMSO solution, which resulted in hindered imidazole tautomerism. The observed hindered tautomerism was studied by 1H NMR spectroscopy. The structures of the prepared ligands were also confirmed by APCI mass spectroscopy. Both chiral amines and tridentate compounds have been applied as ligands in copper (II)-catalyzed nitroaldol reactions (Henry reaction). Various reaction conditions for the Henry reaction have been studied (influence of temperature, molar ratio, solvent or copper (II) precursors). The compounds prepared with the two imidazole rings showed fast reaction times and a reversal in enantioselectivity compared to other chiral amines. 相似文献
258.
259.
The basicities of aluminated zeolites βhave been investigated by FTIR spectra of chemisorbed pyrrole. The NH-stretching frequency of pyrrole adsorbed on the samples shifts towards lower wavenumber as the St/Al ratio is decreased and correlates well with the negative charge on the framework oxygen calculated from the Sanderson electronegativity equalization principle, revealing zeolite β to possess a stronger overall basicity after alumination and, therefore, the alumination to be an effective method to improve the basicity. It is also found that the heterogeneity of basic strength occurs and some stronger basic sites appear after alumination. 相似文献
260.