Efficient microwave induced direct α-halogenation of carbonyl compounds

A novel and direct method for the synthesis of α-halocarbonyl compounds using sequential treatment of carbonyl compounds with [hydroxy(tosyloxy)iodo]benzene followed by magnesium halides under solvent-free microwave irradiation conditions is described.     

A mild and simple synthesis of N-aryl substituted toluenesulfamides under solvent-free conditions

N- aryl substituted benzenesulfamides are often used as heating-sensitive recording material1, thermal printing material2, sensitizer3 and developer4. Moreover, some of the benzenesulfamides have antifungal activities5. Many methods have been described for preparation of sulfamides. They are used to carry out in solvent8 or in solid phase condition9. These methods required solvent or solid support and even required heating or cooling. At the same time, the process of these methods is complex. Now we have developed a new method to prepare N-aryl substituted toluenesulfamides under solvent-free conditions.In recent years, solvent-free technology has gained popularity in organic synthesis. For instance,solidstate reaction and microwave reaction have received considerable attention. Solvent-free synthesis of amides has been reported10-11. This technology has many advantages such as high efficiency and selectivity, easy separation and environmental acceptability. All these merits are in accord with green chemistry's requirements of energy-saving, high efficiency and environmental benefits.In our paper, we used a simple and efficient method for preparing N-aryl substituted toluenesulfamides under solvent-free conditions, as a replacement for classic solvent, which gives many environmental benefits.All reactions were completed at room temperature by co-grinding in an agate mortar for 3-20min and the results are shown in Table 1.In conclusion, we have developed an efficient and convenient method of preparation N-aryl substituted toluenesulfamides in high yields. It symbols an improvement for synthesis of benzenesulfamides.     

Solvent-free Synthesis of Dihydrofuran-fused [60]Fullerene Derivatives by High-speed Vibration Milling

Solvent-free organic reactions have been attracting great interest of chemists due to the elimination of the usage of harmful organic solvents,low costs,and simplicity in the procedure1.Solvent-free mechanochemical reactions of fullerenes were explored and are significant for the reactions of fullerenes because the low solubility of fullerenes in common organic solvents requires large quantity of organic solvents and some novel fullerene reactions could only occur in the solid-state reaction2.…     

无溶剂一锅法合成1,4-二氢吡啶

碳酸氢铵、醛和1, 3-二羰基化合物于70 ℃无溶剂条件下缩合以86～97%的产率得到1, 4-二氢吡啶.     

Synthesis and characterization of surface-cyanofunctionalized poly (N-isopropylacrylamide) latexes

 A series of P[N-isopropylacrylamide (NIPAM)] latexes with different contents of cyano groups were successfully prepared by either seeded or shot-growth polymerizations of an aqueous solution containing acrylonitrile (AN) onto a seed P[NIPAM] latex, respectively, and further characterized by FT-IR, ¹H-NMR, elemental analysis, as well as by quasielastic light scattering (QELS) and scanning electron microscopy (SEM). All prepared surface-cyanofunctionalized P[NIPAM] latexes exhibited the same range of lower critical solution temperature (LCST) as a pure P[NIPAM] latex. The shot polymerization process proved more efficient at yielding cyano derivatized latexes than the seeded polymerization technique. The amount of incorporated cyano groups onto the particles was determined with a good correlation both by ¹H-NMR and elemental analysis. The higher the amount of initially introduced AN monomer in the reaction mixture, the more cyano groups were incorporated onto the particles. The surface of the particles with high content of cyano groups appeared quite rough by SEM in comparison with that of the pure P[NIPAM] particles. Received: 25 February 1998 Accepted: 23 June 1998     

以金属硫酸氢盐为催化剂在无溶剂条件下高效合成3,4-二氢嘧啶-2(1H)-酮

以金属硫酸氢盐M(HSO4)n(Ca(HSO4)2,Zn(HSO4)2和过硫酸氢钾制剂oxone○R)为催化剂催化醛、1,3-二羰基化合物和尿素进行缩合反应,在90℃及无溶剂的条件下高收率、一锅法合成了3,4-二氢嘧啶-2(1H)-酮.     

STUDY ON 1-HEXENE POLYMERIZATION BASED ON ZIEGLER-NATTA CATALYSTS WITH DOPED SUPPORT

A series of Ti/Mg supported catalysts are prepared by using ball-milled mixtures of MgCl2-ethanol adducts and NaCl as supports, and 1-hexene polymerizations catalyzed by the novel catalysts are studied. It is found that the molecular weight distribution of poly(1-hexene) becomes apparently narrower when catalysts with doped supports are used, indicating that changing the structure of the support is an effective way to regulate the active center distribution of heterogeneous Ziegler-Natta catalyst.     

无溶剂研磨条件下四氢苯并吡喃衍生物的一锅法合成

四氢苯并吡喃衍生物在药物和农药研究中有着广泛的用途. 基于合成这类化合物的传统方法所用溶剂多为对环境不利的极性溶剂, 且合成需分步进行, 在提倡绿色化学和发展节约型经济的今天, 如何改良这类反应已成为一个热点. 本工作通过选择不同的碱尝试反应最佳条件, 发现用价廉易得的碳酸钾为碱, 对不同官能团取代的底物芳醛采用研磨的手段, 在无溶剂条件下, 一锅法可成功合成四氢苯并吡喃衍生物. 该法条件温和, 收率高, 易于操作, 对环境影响小.     

Synthesis of 2-imidazolines by co-grinding of N-tosylaziridines and nitriles

1. Download : Download high-res image (74KB)
2. Download : Download full-size image

     

熔融反应合成2,2′-联吡啶桥联二（4,4′-联吡啶）类哑铃型化合物

无溶剂反应;联吡啶;固相熔融;哑铃型化合物