三氟乙酸乙酯的合成工艺优化

Synthesis Process Optimization of Ethyl Trifluoroacetate

三氟乙酸乙酯是合成有机氟化物常用的原料之一,可合成各种含氟农药、医药及其他含氟精细化学品。制备了绿色功能离子液体1-甲基-(3-磺酸基丙基)咪唑硫酸盐[MIM-PS][HSO_(4)]和1-甲基-(3-磺酸基丙基)咪唑对甲苯磺酸盐[MIM-PS][pTSA]作为备选催化剂,以三氟乙酸(TFA)、无水乙醇(AE)为原料,合成三氟乙酸乙酯。考察了催化剂选择、物料比例、催化剂用量、反应时间和反应温度等工艺条件,以及离子液体的重复利用情况。结果表明:当投料质量比例为:m(TFA)∶m(AE)∶m([MIM-PS][HSO_(4)])=5.7∶3.3∶0.4,反应温度为45℃,反应1.5h,产品收率可达98.3%,离子液体催化剂重复利用4次后活性没有明显降低。

Ethyl trifluoroacetate is one of the commonly raw materials for the synthesis of organic fluorides, which can be used to synthesize various fluorine-containing pesticides, medicines and other fluorine-containing fine chemicals. Ethyl trifluoroacetate was synthesized by reaction of trifluoroacetic acid(TFA) with anhydrous ethanol(AE) on pre-prepared catalysts Green functional ionic liquid 1-methyl-(3-sulfonic propyl) imidazolium sulfate [MI-PS][HSO_(4)] and 1-methyl-(3-sulfonic propyl) imidazolium p-toluene sulfonate [MI-PS][pTSA]. The synthesis conditions were investigated, such as catalyst selection, material ratio, catalyst dosage,reaction time and reaction temperature, and the reuse of ionic liquids. The results showed when the mass ratio of feeding was m(TFA)∶m(AE)∶m([MIM-Ps][HSO_(4)]) =5.7∶3.3∶0.4, reaction temperature was 45 ℃ and reaction time was 1.5 h, the yield of ethyl trifluoroacetate could reached 98.3%, and the activity of ionic liquid catalyst does not decrease obviously after being reused for 4 times.