摘要
在无水氯化镁、三乙胺存在下,丁酰氯与丙二酸单乙酯钾盐经缩合、酸解得到丁酰乙酸乙酯;然后与硫脲经脱水、缩合成环后得到6-丙基-2-硫脲嘧啶。结构经1H NMR、IR和MS表征。最佳反应条件为:n(硫脲)/n(丁酰乙酸乙酯)/n(氢氧化钾)=1.00/2.30/2.30时,产物收率为84.71%。本工艺反应条件温和,操作简单,收率高,适合工业化生产。
Based on magnesium chloride and triethylamine catalysis system,ethyl 3-ketohexanoate was synthesized from ethyl potassium malonate and butyryl chloride by acid hydrolysis.After dehydration and cyclization 6-n-propyl-2-thiouracil was got from ethyl 3-ketohexanoate and thiourea.The structure was characterized by 1H NMR,IR,and EI-MS.The yield could arrive 84.71% according to the optimum reaction conditions: material molar ratio of thiourea/ethyl 3-ketohexanoate/potassium hydroxide was 1.00/2.30/2.30.The method is suitable for industry.
出处
《浙江化工》
CAS
2013年第6期10-12,22,共4页
Zhejiang Chemical Industry