1-Methylimidazole → 1-Methyl-3-propylimidazolium iodide

Participants

Reaction Conditions

Reaction Steps

To a 50 ml four necked flask equipped with a stirrer, a dropping funnel, a cooling tube and a thermometer, 41.05 g (0.5 mol) of 1-methyl imidazole and 50 ml of toluene were charged, and heating at 50° C., 93.49 g (0.55 mol) of propyl iodide was dropped slowly taking one hour or more. After stirring under heating at 50° C. for 4 hours, precipitates were separated by filtration, washed by using toluene and dried under a reduced pressure to obtain 122.26 g of 1-methyl-3-propyl imidazolium iodide salt. Then, 122.26 g of the obtained 1-methyl-3-propyl imidazolium methane sulfonate salt was dissolved in 80 ml of water, and a solution in which 139.24 g of lithium bis(trifluoromethane sulfonyl)imide was dissolved in 80 ml of water was added thereto at a room temperature and stirred. From separated two layers, the lower layer was fractionated and by-products were removed by adding 40 wt % of purified water and by water washing five times and vacuum drying was applied to obtain 175.39 g of 1-methyl-3-propyl imidazolium bis(trifluoromethane sulfonyl) imide. As a result of ICP analysis, 2.4 ppm of total alkali metals, 2.9 ppm of chlorine and 6.5 ppm of iodine were contained.

Provenance & Evidence