摘要
以水为溶剂,1,3-环己二酮与甲醛和二甲胺进行Mannich反应,生成2-亚甲基(1,3-环己二酮),该生成物进而与1,3-环己二酮经Michael缩合,得到2,2′-亚甲基双(1,3-环己二酮)粗产物,将其采用弱碱中和的简单分离方法进行提纯,所得最终产物中2,2′-亚甲基双(1,3-环己二酮)纯度为99.8%(质量分数),收率为92.8%;考察了反应温度、时间、pH及提纯用碱的种类对反应产物收率和纯度的影响;最佳制备条件为:20℃2、.5 h、pH=6、弱碱NaHSO3中和,整个制备过程操作简单,成本较低。
2,2＇-Methylenebis （1,3-cyclohexanedione） has been prepared by reaction of 1,3-cyclohexanedione, formaldehyde and dlmethylamine in aqueous solution. The purity of the product （2,2＇-methylcnebis （1,3-cyclohexanedione） is 99.8 %. The yield has been improved from the reported 84.2 % to 92.8 %. The reaction proceeds through the addition of 1,3-cyclohanedione with 2-methylene （1,3-cyclohexanedione）, which results from a Mannich reaction of 1,3-cyclohexanedione, formaldehyde and dimethylamine. The preparation conditions are： reaction temperature 20 ℃; reaction time, 2.5 h; pH = 6; and NaHSO3 as the base.
出处
《化学世界》
CAS
CSCD
北大核心
2006年第5期299-301,共3页
Chemical World
基金
上海市教委重点学科建设基金项目(P1502)
