溫和條件下去丙酮保護(hù)制備末端單炔烴及末端二炔的方法
發(fā)布時(shí)間:2018-10-13 10:50
【摘要】:末端炔烴是有機(jī)合成中重要的原料或中間體.通過(guò)鈀催化的Sonogashira偶聯(lián)反應(yīng),將2-甲基-3-丁炔-2-醇連接到其它基團(tuán)上所得到的結(jié)構(gòu),可以看作是一類丙酮保護(hù)的末端炔烴.目前,對(duì)于這種丙酮保護(hù)的末端炔烴,其去保護(hù)得到端基炔主要是通過(guò)KOH存在下在甲苯中回流數(shù)小時(shí)的方法,但是反應(yīng)溫度高,條件苛刻,適用范圍較窄.對(duì)這一脫保護(hù)過(guò)程進(jìn)行研究,通過(guò)對(duì)多種溶劑和反應(yīng)溫度進(jìn)行對(duì)比,發(fā)現(xiàn)以1,4-二氧六環(huán)作為溶劑,KOH作為堿,可以在相對(duì)較低的溫度(60℃)下得到較高的產(chǎn)率,而且所需時(shí)間大大縮短(0.5~2 h),拓展了這種方法的應(yīng)用范圍.
[Abstract]:Terminal alkynes are important raw materials or intermediates in organic synthesis. By palladium catalyzed Sonogashira coupling reaction, the structure of 2-methyl-3-butyne-2-ol linked to other groups can be regarded as a class of acetone-protected terminal alkynes. At present, for the terminal alkynes protected by acetone, the method of refluxing the terminal alkynes in toluene in the presence of KOH is the main method, but the reaction temperature is high, the conditions are harsh, and the range of application is narrow. Through the comparison of various solvents and reaction temperatures, it was found that the higher yield could be obtained at a relatively low temperature (60 鈩,
本文編號(hào):2268343
[Abstract]:Terminal alkynes are important raw materials or intermediates in organic synthesis. By palladium catalyzed Sonogashira coupling reaction, the structure of 2-methyl-3-butyne-2-ol linked to other groups can be regarded as a class of acetone-protected terminal alkynes. At present, for the terminal alkynes protected by acetone, the method of refluxing the terminal alkynes in toluene in the presence of KOH is the main method, but the reaction temperature is high, the conditions are harsh, and the range of application is narrow. Through the comparison of various solvents and reaction temperatures, it was found that the higher yield could be obtained at a relatively low temperature (60 鈩,
本文編號(hào):2268343
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