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2.3. Characterization The modified clay support and supported Ni0-nanoparticles were characterized by using PXRD, surface area analyzer and transmission electron microscopy (TEM) studies [32]. The powder XRD was recorded in Rigaku Ultima IV machine with Cu Kα radiation (λ=1.5409 Å  .The textural properties measured by using Autosorb-1 (Quantachome,USA) and transmission electron microscopy (TEM) image were recorded on a JEOL JEM-2011 electron microscope.2.4. Synthesis of Hantzsch polyhydroquinoline derivatives To a mixture of aromatic aldehyde (1 mmol), dimedone (1 mmol), ethylacetoacetate (1 mmol), and ammonium acetate (1.5 mmol) in a10 ml round bottom flask, modified Mont. supported Ni0-nanoparticle catalyst (25 mg) was added [Scheme 1]. The mixture was homogenized and stirred at room temperature for 20–25 min, the progress of the re-action was monitored by thin layered chromatography. After comple-tion, 10 ml dichloromethane was added to the reaction mixture; thecatalyst was removed by filtration and washed with dichloromethane and acetone. Then, the liquid portion was extracted with ethyl acetate and water to remove any unreacted ammonium acetate; the organic layer was dried over sodium sulfate and concentrated in vacuum to afford the crude products. The pure product was obtained by recrystal-lization from ethanol. |
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2楼2014-09-24 21:44:02
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2.3.表征 用功率X射线衍射(PXRD)、表面积测定仪和透射电子显微镜（TEM）对改性粘土支撑和支持的NiO纳米颗粒进行表征【32】。用带有铜嘉辐射(λ=1.5409 Å）的Rigaku Ultima IV记录功率X射线衍射(PXRD)结果。使用AUTOSORB-1（Quantachome，美国）测定纹理（结构）特征。用JEOL JEM-2011电子显微镜记录透射电子显微镜（TEM）的影像. 2.4.Hantzsch 多聚羟基喹啉衍生物的合成 向含有混合物芳香醛（1毫摩尔），双甲酮（1毫摩尔），乙酰乙酸乙酯（1毫摩尔）和乙酸铵（1.5毫摩尔）的10毫升混合圆底瓶中加入改性Montmorillonite支持的Nio纳米颗粒催化剂（25毫克）[流程图1]。将混合物均化并在室温下搅拌20-25分钟后，用薄层层析监测反应进程。完成后，向反应混合液加入10毫升二氯甲烷; 用过滤、二氯甲烷和丙酮洗涤方法除去催化剂。然后，用乙酸乙酯和水萃取液体部分，以除去任何未反应的乙酸铵。将有机层用硫酸钠干燥并真空浓缩，得到粗产品。用乙醇重结晶得到纯品。 |
3楼2014-09-25 02:44:32
