蚊蝇醚合成新工艺研究

以2-吡啶酚钠、4-苯氧基苯酚、环氧丙烷和对甲苯磺酰氯为原料,经过三步反应确定了合成蚊蝇醚的最佳工艺条件:1)n(4-苯氧基苯酚)∶n(环氧丙烷)=1∶3.0,反应温度26～30℃,反应时间4h,1-(4-苯氧基苯氧基)-2-丙醇收率可达98.8%;2)n(1-(4-苯氧基苯氧基)-2-丙醇)∶n(对甲苯磺酰氯)=1∶1.3,反应温度6～10℃,反应时间10h,1-(4-苯氧基苯氧基)-2-对甲苯磺酸丙酯收率高达98.1%;3)n(2-吡啶酚)∶n(1-(4-苯氧基苯氧基)-2-对甲苯磺酸丙酯)=1.6∶1,110℃沸腾,反应时间3h,蚊蝇醚收率可达91.0%。用1 H NMR对蚊蝇醚结构进行了表征。

New Synthetic Process of Pyriproxyfen

Pyriproxyfen was prepared using pyridn-2-odsodium,4-phenoxyphenol,propylene oxide and 4-toluene sulfonyl chloride as starting materials through three steps.The obtained optimum conditions and yields for each step were(1) n(4-phenoxyphenol)∶n(propylene oxide)= 1∶3.0,temperature 26—30 ℃and reaction time 4 h,the yield of 1-(4-phenoxyphenoxy)propy-2-ol 98.8%;(2) n(1-(4-phenoxyphenoxy)propy-2-ol)∶n(4-toluene sulfonyl chloride)=1∶1.3,temperature 6—10 ℃ and reaction time 10 h,the yield of PPP-Ts 98.1%;(3)n(pyridn-2-odsodium)∶n(PPP-Ts)=1.6∶1,temperature 110 ℃ and reaction time 3 h,the yield of pyriproxyfen 91.0%.The structure of obtained pyriproxyfen was characterized by 1H NMR.