N-[O,O-二乙基膦酸酯基-(2-羟基苄基)]-2-氨基乙酸钾的微波无溶剂合成及生物活性研究

报道了利用微波无溶剂技术合成化合物N-[O,O-二乙基膦酸酯基-(2-羟基苄基)]-2-氨基乙酸钾的新方法.此方法操作简便,条件温和,反应时间短,环境友好,并对该化合物进行了初步的生物活性研究.     

微波辐射下N-芳基对甲苯磺酰胺的合成

报道了一种合成N-芳基对甲苯磺酰胺的新方法.在微波辐射下,2摩尔比率的芳胺和对甲苯磺酰氯发生反应合成了11个N-芳基对甲苯磺酰胺,该方法操作简便,产率高(84%~97%).     

有机硅浸渍漆研究进展

概述了国内外有机硅浸渍漆的制备研究进展和发展现状,对有机硅浸渍漆的改性方法进行了介绍,展望了有机硅浸渍漆的发展趋势,具有高导热、耐热、耐高压、节能环保等性能的加成型无溶剂有机硅绝缘漆将是未来发展方向.     

9-（4-溴苯基）-3，4，6，7-四氢化-3，3，6，6-四甲基吖啶-1，8-（2H，5H，9H，10H）-二酮的合成和晶体结构

摘要:标题化合物C23H26BrNO2是由4-溴苯甲醛、5,5-二甲基-1,3-环己二酮(哒米酮)和NH4OAc在无溶剂条件下,80℃加热反应而得,结构通过单晶X射线衍射法确定,其晶体属正交晶系,空间群Pna2(1),Mr=428.36,a=1.408 9 nm,c=1.085 6(3)nm,V=2.154 7(9)nm3,Z=4,Dc=1.320 g/cm3,μ=1.924 mm-1,F(000)=888,晶体结构用直接法解出,使用全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.040 2,Rw=0.069 9.     

Green Light-Emitting Region-Regular Poly（9,9-Dihexylfluorene-co-Fluorenone） Prepared from Solvent-Free Oxidative Coupling Polymerization

Soluble green light-emitting poly（9,9-dihexylfluorene- co-fluorenone） was synthesized by solvent-free oxidative coupling polymerization of 9,9-dihexylfluorene in a facile one-step reaction. The polymers were characterized by FT-IR, ^1H NMR, ^13C NMR, UV-Vis and fluorescence spectroscopy. The region-regular structure of the polymer linking at 2, 7＇-position on the fluorene moieties was obtained. The FT-IR spectra of the polymers showed fluorenone vibration. The fluorescence spectra of the solid thin film of the polymers displayed green light-emitting, which was emitted from fluorenone moieties produced in the polymerization process.     

Development of Self-Organized Polymeric Lewis Acid-Catalysts for the Zero-Emission Synthesis of 2-Amino Alcohols

β-Amino alcohols are versatile synthetic intermediates for a wide range of biologically active natural and unnatural products. They can also serve as good chiral ligands for some asymmetric metal complex catalysts. The nucleophilic ring-opening of epoxides with an amine is one of the most efficient routes to obtain such β-amino alcohols with 1,2-trans stereochemistry. Therefore, various homogeneous catalysts have been developed for this transformation. Meanwhile, the development of efficient heterogeneous catalysts that can be easily prepared, recovered, and reused without losing their activities has currently received much attention from a practical and environmental point of view, and not a few such reusable heterogeneous catalysts （e. g. , supported on inorganic materials or insoluble polymers） have been developed. In general, however, they tend to show lower catalytic activities and selectivities compared to the corresponding homogeneous one, and the preparation of them are often tedious.     

固相合成MAPO-5分子筛及其在甲苯催化燃烧中的应用

以二正丙胺磷酸盐(DPA·H₃PO₄)和四乙基溴化铵(TEABr)为双模板剂,采用简单、绿色、高效的固相研磨法合成了多级孔杂原子磷酸铝分子筛CeAPO-5和CoAPO-5;为提升催化性能,增加分子筛中铈离子的含量,制备了一系列不同铈掺杂量的CeAPO-5分子筛,包括CeAPO-5分子筛(w(Ce)=2%)、1.2CeAPO-5分子筛(w(Ce)=2.4%)和2CeAPO-5分子筛(w(Ce)=4%)。通过X-射线衍射(XRD)、扫描电子显微镜(SEM)、N₂吸脱附测试(BET)、固体紫外可见(UV-Vis)漫反射光谱和X射线光电子能谱(XPS)等手段对所合成分子筛进行表征,同时以甲苯为目标污染物,考察了分子筛催化剂在催化燃烧反应中的催化性能。结果表明,所合成的分子筛都具有典型的AFI结构,结晶度较高,且Ce离子和Co离子被成功引入到分子筛骨架中;CeAPO-5分子筛在甲苯催化燃烧反应中较CoAPO-5分子筛具有更好的催化性能;在将金属Ce的含量从2%提高到4%的过程中,催化剂催化氧化甲苯的活性也有所提高,当反应温度为400 ℃时,2CeAPO-5分子筛的甲苯转化率接近100%;通过对催化剂在360 ℃时催化氧化甲苯的稳定性进行研究发现,2CeAPO-5分子筛在经过30 h的反应后仍保持70%左右的甲苯转化率。     

取代-3-甲酰基色酮与麦氏酸的固相缩合反应

在无溶剂无催化剂条件下,采用石蜡油加热的方法,由取代-3-甲酰基色酮与麦氏酸通过Knoeve-nagel缩合反应合成了一系列5-(色酮基-3-亚甲基)麦氏酸类化合物,收率70%~87%,产物结构经IR,1H NMR确认.     

在无溶剂条件下用微波辐射及相转移催化合成肉桂腈

以肉桂醛为原料,在微波辐射及相转移催化剂聚乙二醇-600催化作用下由SiO2/Na2CO3-NaOH混合碱促进的无溶剂一步法直接制备肉桂腈.确定的最佳反应条件是:肉桂醛与盐酸羟胺摩尔比1:1.4～1:1.6;对应每1mmol肉桂醛,SiO2的用量为0.25～0.30 g;催化剂为PEC-600和Na2-NaOH(7:3,摩尔比),彻底研磨后用微波辐射功率为520 W,反应时间为5 min,制备效果最佳.在此条件下,从肉桂醛制备肉桂腈的平均得率达86.9%.