高效卫生杀虫剂丙烯菊酯的合成工艺改进

Improved Synthesis of Allethrin Used as High Effective Hygienic Insecticide

由2-甲基呋喃?三氯氧磷?氯丙烯等为原料经四步反应合成丙烯菊酯.其关键中间体烯丙醇酮是由2-(1-羟基-3-丁烯基)-5-甲基呋喃催化异构合成,并将传统的两步反应简化为一步反应,简化了工艺流程,缩短了反应时间,提高了烯丙醇酮的产率.该中间体产率由文献报道的最大值83.0%提高到88.0%.确定了该中间体的最佳反应条件为:以水为反应介质,m催化剂∶m反应物=3∶100,反应时间23h.与文献报道的其他合成路线相比,该工艺有利于丙烯菊酯的工业化生产.

Allethrin was prepared from 2-methylfuran, phosphoryloxychloride and chloropropene by four-step reaction. Allethrolone was prepared from 2-（ 1-hydroxy-3-butylene）-5- methylfuran via catalytic isomerization, and the traditional two-step reaction was changed into an one-step reaction. As a result, the process was shortened. The optimum process conditions were investigated and it was preferable to perform the reaction in water, mcatalyst：mreactant =3 ： 100 and the reaction was finished in about 23 h. The yield of allethrolone was 88.0%, which was higher than the maximum value 83.0% reported in literature. This method is characteristic of short step, high efficiency etc, compared with other synthetic routes. It makes the industrialization of synthesis of allethrin possible.