单活泼氢手性配体生成的原位镁催化剂及其在不对称合成中的应用

本文对原位镁催化剂近年的工作进行了总结,对由单活泼氢手性配体生成的原位镁催化剂在不对称合成中的应用进行了系统归纳和分类。介绍了由单氮氢键、单酚羟基和单醇羟基构成的手性配体的设计和发展及其在原位镁催化剂中的应用,实现了多种类型的不对称催化反应过程和化学键的形成方式。对于原位镁催化策略的进一步探索,将有助于研究和推广更多类型廉价环保金属资源催化的化学转化过程。     

钴镁铁水滑石的合成、表征及衍生复合氧化物酸碱催化活性研究

以Co(NO3)2.6(H2O)、Mg(NO3)2.6(H2O)和Fe(NO3)3.9(H2O)为原料,以NaOH和Na2CO3为沉淀剂采用低过饱和共沉淀法合成了CoMgFe系列的碳酸根水滑石,通过XRD,IR,TG-DTA,等手段对样品进行测试和表征,X-衍射结果显示,其M2 /M3 投料物质的量比为2-4得到的水滑石为理想构型。经焙烧后,发现其复合氧化物对乙醇催化脱水、脱氢反应有一定的活性。     

Synthesis and Crystal Structure of 3,（5-Amino-4-ethoxycarbonyl-3-methylthio-1-H- pyrazolyl）-5-phenyl-1,2,4-triazine

1 INTRODUCTION Substituted 1,2,4-triazines represent an important class of nitrogen-containing heterocycles. The 1,2, 4-triazine core is a versatile synthetic platform to access a wide range of condensed heterocyclic ring systems via intramolecular Diels-Alder reactions with a vast array of dienophiles[1~5]. In addition, 1,2, 4-triazines have been associated with diverse activi- ties such as antihypertension and inhibition of pla- telets[6] and antiinflammatory[7], and been a key com- po…     

镁及镁合金中微量磷的测定方法研究

磷与钼酸铵形成磷钼杂多酸络幌物,用乙酸丁酯萃取分离,用SnCl2还原反萃取后借磷钼蓝光度法测定镁及镁合金中微量磷。在波长700 nm处工作曲线线性范围0~1.5μg/mL,相关系数为0.9995,络合物表观摩尔吸光系数ε=1.45×104L.mol-1.cm-1,相对标准偏差在1.40%~3.10%之间,加标回收率在99.3%~101.0%之间,本法与ICP法相对照结果比较满意。     

基体分离-电感耦合等离子体原子发射光谱(ICP-AES)法测定精铋中10种杂质元素

采用电感耦合等离子体原子发射光谱(ICP-AES)法测定精铋中Cd、Co、Cu、Fe、Mg、Mn、Ni、Pb、Ti、Zn等十种杂质元素,样品用优级纯硝酸溶解,往60℃左右的溶液中,滴加氨水(1+1),控制pH值在3.0～4.0.考察了温度、酸度、沉降时间对铋的去除率和对检测结果的影响.根据分析线的选择原则,结合待测元素...     

六(乙氧基吡咯烷酮)三聚磷腈的合成与表征

以N-羟乙基吡咯烷酮与氢化钠作用生成相应的钠盐,再将此钠盐与六氯三聚磷腈(HCCP)发生亲核取代反应,合成了六(乙氧基吡咯烷酮)三聚磷腈,用IR、31P NMR、1H NMR、13C NMR、DEPT、FABMS等现代谱学技术对其结构进行了表征。生物活性试验表明,此化合物1mg/mL时对腐生线虫Panagrellus redivivus的72h致死率为52·7%。     

Synthesis and Crystal Structure of a Novel Manganese Coordination Polymer： 2,5-Bis（4-pyridyl）-3,4-diaza-2,4-hexadiene

A new manganese coordination polymer 1, [Mn(H2O)4(L)]n(ClO4)2n·2nH2O·3nL (L = 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene), has been synthesized and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group Pn with a = 13.9176(8), b = 15.4754(9), c = 15.9670(9) , β = 99.5010(10)o, V = 3391.8(3) 3, Z = 2, C56H68Cl2MnN16O14 , Mr = 1315.10, Dc = 1.288 g/cm3, μ = 0.344 mm-1, F(000) = 1374, R = 0.0733 and wR = 0.2035. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene and four oxygen atoms from water molecules, completing an octahedral geometry. The title complex exhibits a novel supramolecular layer architecture sustained by the concurrence of coordination bonds, hydrogen bonds, and π-π stacking interactions.     

Influence of Fe2O3 and V2O5 on Crystalline Structure of Mg-Al Spinel Synthesized by Waste Aluminum Slag

Mg-Al spinel is synthesized by using industrial waste-residue and basic magnesium carbonate in the aluminum factory as the main raw materials. The influence of V2O5 and Fe2O3 mineralizers on the structure, cell parameters and microscopic morphology of synthesized Mg-Al spinel has been discussed. The Mg-Al spinel is characterized by using XRD, SEM and relevant analytical software, such as Philips plus, Rietveld quantification and so on. The experimental results show that certain amounts of V2O5 and Fe2O3 are beneficial to the formation of Mg-Al spinel, and the optimum addition of V2O5 and Fe2O3 is respectively 2wt% and 3wt%. V2O5 has few effects on cell parameters of Mg-Al spinel; but Fe2O3 can form solid solution with Mg-Al spinel in which Mg-Fe spinel can also dissolve to form continuous solid solution. Therefore, with the increase of Fe2O3 content, the cell parameters of Mg-Al approximately present linear increase.     

3-酰基焦脱镁叶绿酸甲酯的格氏反应及其叶绿素衍生物的合成

叶绿素-α衍生物是环状四吡咯化合物,虽然由于D环双键的饱和而隶属于卟吩类化合物,但仍然保持卟啉基所具有的多齿配位作用以及共轭大环的结构表征,其中,连带多种有机官能团的非对称性氮杂轮烯结构、A-B环端的亲脂溶性和C-D环端亲水溶性以及稠并的五元E-环,均明显影响着叶绿素衍     

偏硼酸钙改性al-mcm-41催化剂的表征及催化性能

al-mcm-41分子筛;偏硼酸钙;催化性能;乙氧基化