丙炔[口恶]草酮的合成新方法

New Process for the Synthesis of Oxadiargyl

[目的]研究一种温和、安全性好的丙炔[口恶]草酮合成新方法。[方法]以无水碳酸盐为缚酸剂,在DMF溶剂中,5-特丁基-3-[2,4-二氯-5-羟基苯基]-1,3,4-[口恶]二唑-2(3H)-酮与对甲苯磺酸炔丙基酯反应合成丙炔[口恶]草酮,探究了实验条件对反应的影响。[结果]以对甲苯磺酸炔丙基酯替代燃爆性强的3-氯丙炔,在常压、无催化剂条件下合成丙炔[口恶]草酮,收率最高为97.1%,溶剂回收可循环使用。

[Aims]This paper aims to study a mild method with good safety for the synthesis of oxadiargyl.[Methods]The effects of experimental conditions on the reaction were investigated by the reaction of 5-tert-butyl-3-[2,4-dichloro-5-hydroxyphenyl]-1,3,4-dihydro-2-(3H)-one with propargyl p-toluene sulfonate in DMF solvent with anhydrous carbonate as acid-binding agent.[Results]Propargyl p-toluene sulfonate was used instead of flammable and explosive 3-chlorpropargyne to synthesize oxadiargyl at atmospheric pressure without catalyst.The highest yield was97.1%and the solvent could be recycled.