4-甲氧基-3-丁烯-2-酮的合成工艺

A NOVEL SYNTHESIS OF 4-METHOXY-3-BUTENE-2-ONE

以丙酮(DMK)与甲酸甲酯(MF)为原料,甲醇钠为催化剂,通过缩合反应制备了乙酰基甲氧基乙醇钠盐,经酸性条件下脱水得到4-甲氧基-3-丁烯-2-酮(MVK),产物结构经~1H NMR及MS进行了表征。通过单因素、正交实验和放大重复性实验确定了最佳反应条件,结果表明:以甲醇钠为催化剂,四氢呋喃为溶剂、n(甲醇钠)∶n(MF)0.9∶1,n(DMK)∶n(MF)为1.5∶1,30℃反应12 h,在此条件下,平均收率达86.9%。

4-Methoxy-3-buten-2-one(MVK)was synthesized by aldol condensation using acetone(DMK)and methyl formate(MF)as raw materials,sodium methoxide as catalyst and tetrahydrofuran as solvent.The molecular structure of the product was confirmed by~1H NMR and MS.The optimal reaction conditions were determined by single factor orthogonal experiments and repeated scale-up experiments.The optimum reaction conditions are:sodium methoxide as catalyst,tetrahydrofuran as solvent,n(sodium methoxide)∶n(MF)=0.9∶1,n(DMK)∶n(MF)=1.5∶1,30℃for 12 h.MVK was obtained with an average yield of 86.9%under the optimal reaction conditions.