4,4-二甲氧基-2-丁酮的合成研究

以金属钠为原料,甲醇为溶剂,先制成甲醇钠的饱和甲醇溶液,再滴加丙酮和甲酸甲酯进行Claisen酯缩合制得丁酮烯醇钠,最后在强酸作用下与甲醇进行缩醛化反应合成了4,4-二甲氧基-2-丁酮,过程总收率达到73.1%,纯度98.7%。产品通过IR和MS进行了表征。考察了原料的用量、反应温度,反应时间、滴加速度、反应体系pH值等方面对反应收率的影响,并得出了最适宜的工艺条件。

Synthesis of 4,4-Dimethoxy-2-butanone

4,4-Dimethoxy-2-butanone was synthesized through three-step process using sodium and methanol as the starting material.Firstly,the methanol solution of sodium methoxide was prepared.Secondly,a mixture of acetone and methyl formate was added into the methanol solution of sodium methoxide to prepare sodium formyl acetone by Claisen reaction.Lastly,4,4-dimethoxy-2-butanone was prepared through acetylizing reaction in methanol solution with sulfuric acid.The overall yield reached(73.1%) and the purity of the the product was 98.7%.The product was confirmed by IR and MS.Meanwhile,the effect of ratio of materials,temperature,reaction time,feeding speed and pH value on the reaction was investigated,and the optimum reaction conditions were obtained.