酸性功能化离子液体催化合成苹果酯及其同系物

Synthesis of fructone and its derivatives by using acidic ionic liquid as catalyst

制备了一种吡嗪型酸性功能化离子液体,1-(4-磺酸基)丁基-3-甲基吡嗪四氟硼酸盐([4-Sulfbmpyrazine][BF4]),并以其为酸性催化剂,合成了苹果酯及其同系物,采用正交实验方案对合成条件进行了考察,实验结果表明,以[4-Sul-fbmpyrazine][BF4]为催化剂合成苹果酯的较优条件为:反应物物质的量比n(乙酰乙酸乙酯)∶n(乙二醇)=0.10∶0.15,反应时间8 h,催化剂用量0.5 g,带水剂用量40 mL,按优化条件进行验证实验,产品得率为95.4%。按上述实验方法合成了一系列苹果酯同系物,实验均取得了良好的效果。而且催化剂循环使用5次,催化活性基本不变。可为苹果酯及其同系物的合成提供一条较为优化、绿色的合成新途径。

The acid functional ionic liquid 1-（4-sulfobutyl）- 3-methylpyrazinium tetrafluoroborate （ abbreviated as [ 4-sul- fbmpyrazine] [ BF4 ] ） ,was prepared. Fructone and its deriva- tives were prepared by the reaction of ethyl acetoacetate and diol in the presence of [ 4-sulfbmpyrazinel [ BF4 ] as acidic catalyst. And the proper technological conditions were identified as follows by orthogonal experiments. The proper reaction conditions of fructone is a ratio of tool n（ethyl acetoacetate） ： n （ethylene glycol） = 0.10： 0.15, the reaction time of 6 h, the amount of catalyst of 0. 5 g and the amount of cyclohexane as carrying-water reagent of 40 mL. The yield could reach 95.4%. Six kinds of derivatives of fructone are synthesized using acidic functional ionic liquid as catalyst. The catalyst had a fairly high catalytic activity and high yield. The acidic functional ionic liquid could be recovered and reused for at least five times without the loss of efficiency. It provided a new and green way for the synthesis of Fructone and its derivatives.