1-Methylimidazole → 1-Methyl-3-propylimidazolium Iodide

Temperatur

50 °C

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.

1. waittaking one hour or more
2. temperatureunder heating at 50° C. for 4 hours
3. customprecipitates
4. customwere separated by filtration
5. washwashed
6. customdried under a reduced pressure

ORD-Eintrag

ord-5c8f7a90ace04aaf89fae2bfff1d85f5

Quelldatensatz

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07605271B2