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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. |
金蟲 (小有名氣)
至尊木蟲 (知名作家)
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2.3.表征 用功率X射線衍射(PXRD)、表面積測定儀和透射電子顯微鏡(TEM)對改性粘土支撐和支持的NiO納米顆粒進行表征【32】。用帶有銅嘉輻射(λ=1.5409 Å)的Rigaku Ultima IV記錄功率X射線衍射(PXRD)結果。使用AUTOSORB-1(Quantachome,美國)測定紋理(結構)特征。用JEOL JEM-2011電子顯微鏡記錄透射電子顯微鏡(TEM)的影像. 2.4.Hantzsch 多聚羥基喹啉衍生物的合成 向含有混合物芳香醛(1毫摩爾),雙甲酮(1毫摩爾),乙酰乙酸乙酯(1毫摩爾)和乙酸銨(1.5毫摩爾)的10毫升混合圓底瓶中加入改性Montmorillonite支持的Nio納米顆粒催化劑(25毫克)[流程圖1]。將混合物均化并在室溫下攪拌20-25分鐘后,用薄層層析監(jiān)測反應進程。完成后,向反應混合液加入10毫升二氯甲烷; 用過濾、二氯甲烷和丙酮洗滌方法除去催化劑。然后,用乙酸乙酯和水萃取液體部分,以除去任何未反應的乙酸銨。將有機層用硫酸鈉干燥并真空濃縮,得到粗產(chǎn)品。用乙醇重結晶得到純品。 |
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