西瓜酮的合成与纯化  

Synthesis and Purification of Calone

作　　者：岳智洲[1] 梁玉坤[1] 

机构地区：[1]武汉理工大学化学工程学院,湖北武汉430070

出　　处：《广州化工》2013年第9期80-81,276,共3页GuangZhou Chemical Industry

摘　　要：以4-甲基邻苯二酚和1,3-二氯丙酮为原料,以碳酸钠为碱,碘化钾为催化剂;经过环合,得西瓜酮粗品。此粗品与盐酸羟胺反应得到西瓜酮粗品,再通过重结晶得到高纯度的西瓜酮肟。西瓜酮肟用亚硫酸氢钠氧化室温脱肟得到高纯度的西瓜酮。确定了最佳反应条件,总收率为50%。化合物结构通过1H NMR和13C NMR进行了表征。The crude calone was synthesized from 4 - methylcatechol and 1,3 - dichloroacetone in the presence of sodium carbonate and potassium iodide via cyclization. The crude calone was reacted with hydroxylamine hydrochloride to give crude calone oxime. The crude calone oxime was purified via recrystallization to give calone oxime with high purity. The calone with high purity was obtained with sodium bisulfite agents via oxidizing deoximation. The optimal reaction conditions were confirmed and the total yield was 50%, The target product was characterized by ^1H NMR and ^13C NMR.

关 键 词：西瓜酮 4-甲基邻苯二酚 1 3-二氯丙酮 西瓜酮肟 亚硫酸氢钠 

分 类 号：TQ657.2[化学工程—精细化工]