2-氨基-4-溴-5-氯苯甲酸的合成

以硝基苯为原料，经溴化、还原、缩合、环合、氯化和氧化等６步反应合成了２－氨基－４－溴－５－氯苯甲酸，总收率为１１．７％。     

水杨醛型腙类试剂测定铝的研究

合成了以水杨醛为母体的４种腙类新荧光试剂，并对其与铝的荧光反应性能进行了比较研究，结果表明，５－溴－水杨醛水杨酰腙是一种优良试剂。它与铝在ｐＨ５．４醋酸－醋酸铵缓冲溶液中形成１３型荧光配合物，其λｅｘ＝３７０ｎｍ，λｅｍ＝４６０ｎｍ。建立的分析方法检测下限为１．１ｎｇ／ｍＬ，相对标准偏差为１．４５％。考察了３０余种共存离子的干扰情况。直接应用于葡萄糖注射液及常见饮料中微量铝的测定，结果满意。     

单溴四苯基卟啉吸附在AgCl溶胶表面性质研究

合成了单溴四苯基卟啉—— 5 - (邻溴苯基 ) - 1 0 ,1 5 ,2 0 -三苯基卟啉 (H2 L) ,用元素分析 ,红外光谱、电子吸收光谱和氢核磁共振谱确定了其组成和结构。研究了 H2 L在醋酸中电子吸收光谱和在 Ag Cl溶胶上的表面化学反应。结果表明 ,单邻溴四苯基卟啉在冰醋酸中以二酸形式 H4 L2 + 和游离碱 H2 L形式存在 ,二者之间存在着电离平衡 :H4 L2 + =H2 L+2 H+ ;当 p H=7.0～ 1 1 .0时 ,H2 L在Ag Cl溶胶表面发生配位反应生成 Ag( ) L,并且溶液的 p H增大 ,配位反应的速率增大。     

6-溴-2-萘酚和2-萘酚的HPLC同时测定

采用高效液相色谱法同时测定了6-嗅-2-萘酚和2-萘酚的含量。用SHIMPACK CLC ODS色谱柱,甲醇+0.05％磷酸水溶液=70+30为流动相,UV检测器,检测波长为275nm;6-溴-2-萘酚的线性范围为0.01 mg·ml-1-1.0 mg·ml-1,r=0.9993,平均回收率为99.8％。2-萘酚的线性范围为0.0001 mg·ml-1 -0.005mg·ml-1,r=0.9991,平均回收率为98.1％,该法准确、简便,可用于6-溴-2-萘酚的质量控制。     

聚丙烯酸五溴苄基酯及其中间体的研究进展

介绍了聚丙烯酸五溴苄基酯的合成步骤、分子结构和性能特点。并综述了其合成方法及性能的研究进展。     

双子季铵型表面活性剂合成工艺与性能表征

论文研究了采用四甲基丙二胺和溴代十二烷,在异丙醇作为溶剂的条件下合成双子表面活性剂C12-3-C12.2Br。采用红外光谱测定、熔点测定法对合成产物进行表征,并探讨不同反应时间、反应温度、反应物料比对生成产物的影响,同时还检测了产物的表面张力、临界胶束浓度等性质。实验结果表明,所合成的双子表面活性剂的产率是在12 h内随反应时间的增长而增大;在本实验条件下,反应温度对产率的影响就比较小;溴代十二烷过量更有利于反应进行,但过量太多也不利于反应的进行。测定表面张力可知产品的临界胶束浓度(CMC)是1.58mmol/L-1。     

Arylethyne Bromoboration–Negishi Coupling Route to E‐ or Z‐Aryl‐Substituted Trisubstituted Alkenes of ≥98% Isomeric Purity. New Horizon in the Highly Selective Synthesis of Trisubstituted Alkenes

The hitherto unprecedented palladium‐catalyzed cross‐coupling of (Z)‐β‐bromo‐β‐arylethenylboranes can be made to proceed satisfactorily through (1) the use of highly catalytically active bis(tri‐tert‐butylphosphine)palladium or dichloro[N,N‐bis‐(2,6‐diisopropylphenyl)imidazol‐2‐yl](m‐chloropyridine)palladium and (2) conversion of the dibromoboryl group to the (pinacol)boryl group. Thus, a wide variety of carbon groups can be used to substitute bromine in ≥98% stereo‐ and regioselectivity, while suppressing the otherwise dominant β‐debromoboration. Together with the alkylethyne‐based protocols, the alkyne bromoboration–Negishi coupling tandem process has emerged as the most widely applicable and highly selective route to trisubstituted alkenes including those that are otherwise difficult to access.     

离子选择电极法测定有机分析试剂的纯度

利用金属离子与配位体形成ｎ：１配合物,以金属离子选择电极为指示电极,饱和甘汞电极为参比电极,通过直接测定游离金属离子的活度,建立了测定有机分析试剂纯度的新方法。方法简便可靠,用于２－「（５－溴－２－吡啶）偶氮」－５－苯酚和铬天青Ｓ纯度的测定,获得了满意的结果。     

Cure Kinetics and Thermal Properties of Octa(aminophenyl)-POSS/Bromobisphenol A Epoxy Resin Nanocomposites

The tetrabromobisphenol A epoxy resin (TBBPAER) was synthesized and Octa(aminophenyl) polyhedral oligomeric silsesquioxane (OAP-POSS) was used as a curing reagent of TBBPAER. The cure kinetics, the glass transition temperature, and the flame resistance of OAP-POSS/TBBPAER nanocomposites were investigated. The results show that the curing reaction could be described by the autocatalytic ?esták-Berggren (S-B) model. The average activation energy E _a is 129.59 KJ/mol, the maximal mechanical loss temperature (T _p) is 166°C, when the molar ratio (N _s) of amino group to epoxy group is 0.5. The oxygen index for fire resistance is 46 ～ 49 for different amounts of OAP-POSS.     

Study on fluorescence properties of rare earth complexes influenced by steric effect

The rare earth complexes Tb(o-BrBA)3,Tb(m-BrBA)3 and Tb(p-BrBA)3 were synthesized using o-,m-,p-bromo benzoic acids(2-bromo benzoic acid,3-bromo benzoic acid and 4-bromo benzoic acid) as ligand,respectively.The UV spectra showed that the absorption ability of Tb(m-BrBA)3 was the strongest.However,the fluorescent intensity of Tb(o-BrBA)3 was the weakest.The effect of the molecular structure,the energy level of Tb3+ and energy transfer efficiency from ligands to Tb3+ were discussed to explain the experimental results.The results indicated that,due to the large atomic radius of bromine,the steric effect caused by the different substitution bromine on the benzene ring might strongly affect the bond length formed by the coordination atoms and Tb3+.The longer the bond length was,the lower the efficiency of energy transfer was,and the weaker the fluorescent intensity was.