摘要
文章介绍以氰乙酸甲酯为原料,经环合、亚硝化、还原、闭环、硫代和氯代等6步反应合成了2,6-二氯嘌呤,多步操作经简单处理即投下一步反应,对影响反应的关键原料、原料颗粒大小、反应温度及溶剂等进行了探讨,总收率为30%~32%,用红外光谱、紫外光谱对产品进行了结构确证,并用高效液相色谱进行了质量分数测定,此工艺适合工业化生产。
2,6-Dichloropurine was prepared from methyl cyanacetate by the reactions of cyclization, nitrosylation, reduction, closed ring action, thionation and chloration. There are many processes simply dealt with to the next reaction, so the process of the whole reaction was rather simple. The factors that effect the reaction are discussed, including the key raw materials, the size of the particles, the temperature and the solvent of reaction. The total yield was 30%~32%. The target compound was analyzed by IR and UV to make sure it is 2,6-dichloropurine and the assay of the product was measured by HPLC. The technology was suitable for industrial production.
出处
《合肥工业大学学报(自然科学版)》
CAS
CSCD
北大核心
2006年第6期680-682,共3页
Journal of Hefei University of Technology:Natural Science