离子液体N-丁基吡啶四氟硼酸盐的合成研究

Study on the synthesis of ionic liquid N-butylpyridine tetrafluoroborate

由吡啶、溴代正丁烷和四氟硼酸钠为原料合成了标题化合物。首先合成中间体溴代N-丁基吡啶(BPyBr)用正交实验法对反应条件进行了优选,确定了最佳的合成工艺条件为n(吡啶)∶n(溴代正丁烷)=1∶1.2,温度75℃,时间12 h,溶剂20 mL乙腈。在此条件下,产率94.9%。中间体再经过阴离子交换,得到了目标化合物BPyBF4,同样用正交实验法对反应条件进行了优选,确定了最佳的合成工艺条件为n(BPyBr)∶n(NaBF4)=1∶1,温度40℃,时间24 h,溶剂30 mL丙酮。在此条件下,产率99.6%。产物的结构经1HNMR确认。

N-Butylpyridine tetrafluoroborate （ BPyBF4 ） was syn- thesized from pyridine, 1-bromobutane and sodium tetrafluoroborate. Firstly, N-butylbromopyridine （BPyBr） was synthesized as the intermediate. And the proper technological conditions were identified as follows by orthogonal experiments, namely：a ratio of n（Pyridine） ： n （1-bromobutane） = 1 ： 1.2, an amount of solvent acetonitrile of 20 mL, a reaction temperature of 75 ℃ , and a reaction time of 12 h. The yield of BPyBr could reach 94.9% . Then, the target compound BPyBF4 was obtained through anion exchange, and the proper technological conditions were identified as the same shown above, i. e. ： a ratio of n （BPyBr） ： n （NaBF4） =1 ： 1, a reaction temperature of 40 ℃, a reaction time of 24 h, and a dosage of solvent acetone of 30 mL. Under such conditions, the yield of BPyBr could reach 99.6% and the product structure was confirmed by ^1HNMR analysis.