2,3-二氰基丙酸乙酯的合成工艺研究

Studies on the Synthetic Technology of Ethyl 2,3-dicyanopropionate

对氟虫腈的重要中间体——2,3-二氰基丙酸乙酯的合成工艺进行了深入的研究。以氰乙酸乙酯,氰化钠,多聚甲醛为原料进行一步合成反应,对反应的最佳条件和合理的后处理方法进行了摸索,确定最佳反应温度为30℃,反应时间4h,采用先酸化后水洗的后处理方法。收率达85.3%,产品质量分数为92.1%。

Deep studies were made in this paper on the synthetic technology of the important intermediate of fipronil-ethyl 2,3-dicyanopropionate. It was synthesized by one-step reaction with ethyl cyanoacetate,sodium cyanide and paraformaldehyde. After determining the optimal condition and the method of post-treatment 30 ℃ for 4 h and acidification first,the yield can reach 85.3%,and the purity(by GC)was 92.1%.