10-十一烯酸四氟丙酯的合成及表征

Synthesis and characterization of 10-undecenoic acid tetrafluoropropyl ester

以四氟丙醇和10-十一烯酸为原料,采用直接酯化法合成了10-十一烯酸四氟丙酯(UATE),通过FT-IR和1H NMR对UATE进行了结构表征,考察了反应温度、四氟丙醇用量、催化剂用量、甲苯用量及反应时间5个因素对UATE酯化率的影响。通过响应面实验设计对UATE合成工艺进行优化,确定其最佳合成工艺条件为:n(四氟丙醇)∶n(10-十一烯酸)=3∶1,催化剂浓硫酸用量为0.5%,甲苯用量为7.6 m L,反应时间10 h,反应温度为138℃,在该条件下UATE酯化率最大为78.6%。

10-Undecenoic acid tetrafluoropropyl ester （UATE） was synthesized from 2,2,3,3-tetrafluoro-1-propanol and 10-undecenoic acid by direct esterification. The UATE was characterized by FT-IR and 1H NMR. The effects of the reaction temperature, the amounts of tetrafluoropropanol, catalyst and toluene and the reaction time on the yield of UATE were studied. The synthesis process of UATE was optimized through the response surface experimental design. Thus the optimal conditions of synthesis are determined：n （2,2,3,3-tetrafluoro-1-propanol） ： n (10-undeeenoic acid） = 3：1 ; the amount of concentrated sulfuric acid is 0.5% ;the amount of toluene is 7.6 mL;the reaction time is 10 h;the reaction temperature is 138℃. Under such condition,the maximum yield of UATE is 78.6%.