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出 处:《浙江工业大学学报》2016年第3期351-354,共4页Journal of Zhejiang University of Technology
摘 要:研究了一种红外加热辅助固相研磨合成呋喃衍生物的方法,此法绿色无溶剂,方便易操作.通过筛选不同的酸性催化体系及反应条件,发现H2SO4(30%)/SiO2作为催化剂,无需任何溶剂,由1,4-二羰基化合物在红外加热(控温80℃左右)辅助固相研磨条件下,发生Paal-Knorr缩合反应,高效地合成出了一系列呋喃衍生物.同时验证,该方法适用于不同取代基的1,4-二羰基化合物的Paal-Knorr缩合反应.此方法操作简单方便,条件温和可控,反应时间短(6~30min),分离收率高(83%~100%),产物纯度高.A method for the synthesis of furan derivatives by infrared heat aided solid state grinding has been developed.The method can be operated conveniently and easily without solvent.Through screening of different acid catalysts and reaction conditions,a series of furan derivatives were synthesized from 1,4-diketones viasolvent-free Paal-Knorr reaction catalyzed by H2SO4(30%)/SiO2 under infrared heat(the temperature about 80 oC)aided solid state grinding conditions.This method is verified that it is suitable for the Paal-Knorr condensation reaction of1,4-diketones with different substituents.The advantages of this method are simple procedure,mild conditions,rapidity(6~30min),high isolated yields(83%~100%)and high purity.
关 键 词:红外加热 研磨 Paal-Knorr反应 呋喃衍生物
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