3,3-二氟环丁烷羧酸的合成工艺研究

Study on Synthesis Technology of 3,3-Difluorocyclobutanecarboxylic Acid

以3-氧代环丁烷甲酸乙酯为原料,通过路易斯酸催化剂三氟化硼乙醚催化羰基的亲核加成,再经过脱硫氧代反应合成3,3-二氟环丁烷甲酸乙酯,在碱性条件下水解得到最终产物3,3-二氟环丁烷羧酸。此反应路线较短,原材料性能稳定安全,反应条件温和,适合工业化生产。试验得出较佳制备工艺条件:反应时间3 h,反应温度60℃,氢氧化钠最适宜的浓度为1.2 mol/L。

Using ethyl 3-oxocyclobutanecarboxylate as raw material,3,3-difluorocyclobutanecarboxylate was synthesized by nucleophilic addition of carbonyl group catalyzed by Lewis acid catalyst boron trifluoride ether,and then through desulfurization oxo reaction.The final product 3,3-difluorocyclobutanecarboxylic acid was obtained by hydrolysis under alkaline conditions.The reaction route is short,the raw material properties are stable and safe,and the reaction conditions are mild,which is suitable for industrial production.The best preparation process conditions were obtained from the test:the reaction time was 3 h,the reaction temperature was 60℃,and the optimum concentration of sodium hydroxide was 1.2 mol/L.