采用1-溴代己烷和N-甲基咪唑为原料,微波辅助快速合成了溴化1-己基-3-甲基咪唑 ([HMIM]Br)中间体,此步反应产率可达到95%.通过将中间体和六氟磷酸钾进行离子交换,制备了离子液体1-己基-3-甲基咪唑六氟磷酸盐([HMIM]PF_6),产率约为48%.与传统方法相比,反应时间极大地缩短.产物的结构经傅立叶变换红外光谱(FT-IR)、超导脉冲傅立叶变换核磁共振氢谱(~1HNMR)和超导脉冲傅立叶变换核磁共振碳谱(~(13)CNMR)确认,纯度经高效液相色谱法(HPLC)分析达到99.0%以上.
The intermediate 1-hexyl-3-methylimidazolium bromide ([HMIM]Br) was synthesized from N-methylimidazolium and 1-hexylbromide under microwave radiation,and 1-hexyl-3-methylimidazolium hexafluorophosphate ( [HMIM]PF_6) was then prepared using [HMIM]Br and KPF_6 by anion exchange.Compared with traditional methods,the reaction time required was greatly reduced.The structure of the synthesized product was confirmed by FT-IR,~1HNMR and ~(13)CNMR,and the purity of the product was determined to be above 99.0% using high performance liquid chromatography.
参考文献
| [1] | Huddleston J G;Viser A;Reichert W M .[J].Green Chemistry,2001,3:156-164. |
| [2] | 黄明华,马晓国,黄蓓.离子液体及其在环境污染物分离分析中的应用[J].理化检验-化学分册,2007(11):982-986. |
| [3] | Huddleston J G;Willauer H W;Swatioski R P et al.[J].Chemical Communications,1998,18(16):1765-1766. |
| [4] | Volker P;Bohm W;Jlerrmann W A .[J].Chemistry-A European Journal,2000,6(06):1017-1025. |
| [5] | Zhang Z X;Xiong G H;Li G K et al.[J].Analytical Sciences,2000,16(02):221-244. |
| [6] | 赵静,马晓国,黄明华.微波辅助萃取技术及其在环境分析中的应用[J].中国环境监测,2008(06):27-32. |
| [7] | Namboodiri V V;Varma R S .[J].Tetrahedron Letters,2002,43(31):53815383. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%