酸性功能化离子液体催化合成风信子素的研究

Synthesis of acetaldehyde ethyl phenylethyl acetal catalyzed by acidic ionic liquids

通过两步合成法制备得到酸性离子液体1-(4-磺酸基)丁基-3-甲基咪唑四氟硼酸盐,考察了投料物质的量比、反应时间等不同反应因素对其合成的影响,得到最佳反应条件即为投料物质的量比n(N-甲基咪唑)∶n(1,4-丁烷磺内酯)=0.08∶0.1、反应时间为6.5 h、投料物质的量比n(磺基内盐)∶n(氟硼酸)=0.08∶0.1,并对其表征确证,将其作为酸性催化剂,用于风信子素的合成。以常规试剂乙缩醛和苯乙醇为原料,通过醇交换法,一步合成了风信子素,并对其进行正交试验研究。结果表明,合成风信子素的最佳条件为:反应时间6 h、催化剂用量0.6 g、投料物质的量比n(苯乙醇)∶n(乙缩醛)=1∶5、反应温度40℃,收率81.96%。影响风信子素合成收率因素的主次顺序为:反应温度>反应时间>投料物质的量比n(苯乙醇)∶n(乙缩醛)>催化剂使用量,产物结构通过GC-MS和1HNMR进行了表征。

Acidic ionic liquid of 1 - （ 4-sulfo ） -butyl-3-methyltetrat luoroborate was synthesized via two steps and the effects of reactant ratio, reaction time on the synthesis were investiga- ted. The optimum reaction conditions are as follows： ratio of N-methyl imidazole to 1, 4-Butanesultone is 0.08：0. 1 （tool）, reaction time is 6.5 h, ratio of sulfoni~ salt to fluoro- boric acid is 0.08：0.1 （tool）. The ionic liquid was used as the catalyst for the synthesis of hyacinth body through the al- cohol exchanging method using acetal and phenethyl alcohol as the starting materials. The optimum reaction conditions were obtained by the orthogonal test. Reaction time is 6 h, cat- alyst dosage is 0. 6 g, ratio of phenethyl alcohol to acetal is 1 ： 5 （tool） and reaction temperature is 40 =C. The main fac- tors order was reaction temperature 〉 reaction time 〉 reactant ratio 〉 catalyst usage. The hyacinthol structure was confirmed by GC-MS and 1 HNMR.