钒(V)配合物催化羰基化合物一锅法合成氧肟

S. D. Kurbah
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引用次数: 0

摘要

合成了一种产率高的环保型催化剂,并采用多种理化技术对其进行了表征。采用泥浆法合成肟,考察了该环保配合物的催化性能。使用简单的方法成功地进行了催化研究。该工艺具有成本效益高、操作简单、产率高、反应时间短、反应条件温和等优点。以五氧化二钒与腙配体按1:1的摩尔比反应制得配合物,加入碳酸钾(0.14 g, 1 mmol)磨成细黄色粉末。通过底物、15% H2O2、氨和钒(V)络合物的反应进行了模拟。这种反应在臼中进行,然后磨成细粉。反应完成后,用二氯甲烷/水以1:2,v/v萃取粗产物,真空蒸发干燥。我们用新合成的络合物作为催化剂合成了不同种类的肟。通过1H NMR和13C NMR对产物进行了表征。通过检查醛质子的完全消失和肟质子的出现来监测反应的完成。我们还培养了一些产品的单晶,为产品的形成提供了进一步的支持证据。以{[K(h2o)3][V(O)2L]}2为催化剂,在浆料条件下定量制备了各种羰基化合物的肟化反应。催化反应可以在温和的条件下进行,易于扩展,操作步骤简单,使本方案更环保,是合成肟类化合物的较好替代方法。
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One Pot Synthesis of Oximes from Carbonyl Compounds Catalysed by Vanadium(V) Complex
An eco-friendly catalyst was synthesized in good yield and characterized by various physicochemical techniques. The catalytic performance of the environmentally benign complex was investigated via slurry synthesis of oximes. The catalytic studies were successfully carried out using a simple protocol. The fascinating advantage of this protocol is cost effectiveness, simple work up, good yield, short reactions time, and milder reaction conditions. The complex was prepared by reaction of vanadium pentoxide with hydrazone ligand in 1:1 molar ratios, and to this reaction mixture, potassium carbonate (0.14 g, 1 mmol) was added and ground till fine yellow colour powder appeared. Oximations were carried out by reacting the substrates, 15 % H2O2, ammonia and vanadium(V) complex. The reaction was taken in a mortar and ground till a fine powder appeared. After completion of the reaction, the crude product was extracted using dichloromethane/water in 1:2, v/v, evaporated and dried under vacuum. We synthesized different varieties of oximes using our newly synthesized complex as a catalyst. The products were characterized by 1H NMR and 13C NMR spectroscopy. The completion of the reaction was monitored by checking the complete disappearance of the aldehyde proton and the appearance of oxime protons. We also grew some single crystals of the products to provide further supporting evidences about the formation of products. Oximation of various carbonyl compounds was prepared quantitatively under the slurry condition, using {[K(H¬2O)3][V(O)2L]}2 as a catalyst. The catalytic reactions can be carried out under mild conditions, with ease of scalability, and straightforward work-up procedure, which makes the present protocols greener and better alternative methods for the synthesis of oximes.
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