微波法合成烷基吡啶类离子液体

Microwave assisted synthesis of alkyl pyridinium ionic liquids

以吡啶和溴代正丁烷为原料采用微波法合成了中间体溴化N-丁基吡啶([BPy]Br),并通过正交试验对反应条件进行了优化。考察了原料配比、反应时间、微波功率对该反应的影响,结果表明:原料摩尔比1︰1.1时,微波功率在400 W,反应时间20 min为较佳的反应条件。中间体在微波辐射下经过离子交换合成了N-丁基吡啶四氟硼酸盐([BPy]BF4)和N-丁基吡啶六氟磷酸盐([BPy]PF6)。产物结构由IR和1HNMR确证。

In this paper, N-butyl pyridinium bromide （[BPy]Br） as intermediate was synthesized by reaction of pyridine with 1-butyl bromide, orthogonal design method was employed to optimize conditions of the reaction.Then the effects of material ratio,reaction time and microwave power on the yield of [BPy]Br were investigated,the results showed that the best reaction conditions were described as following： the molar ratio of the reaction material wasl：1.1,the power of microwave was 400 W,the reaction time was 20 min.After ion exchanging under microwave irradiation, N-butyl pyridinium tetrafluoroborate（[BPy]BF4） and N-alkyl pyridinium hexafluorophosphate （[BPy]PF6） were obtained. The structures of products were characterized by IR and ^1HNMR.