반응 #2444878

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lithium bis(trifluoromethanesulfonyl)amide

1-ethyl-3-methylimidazolium chloride

charcoal

→

1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide

수율 87.0%

용매

water

water

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후처리

1. 1
   온도The solution was cooled to room temperature
2. 2
   여과filtered
3. 3
   workup.ADDITIONTo the yellow filtrate was added
4. 4
   온도the solution was then heated for a further 24 hours at 65° C
5. 5
   온도to cool to room temperature
6. 6
   여과filtered
7. 7
   기타to give a colorless solution
8. 8
   기타had formed
9. 9
   기타The bottom layer was separated
10. 10
    세척washed three times with deionized water (100 mL)
11. 11
    온도The layer was then heated at 65° C. under vacuum for 48 hrs
12. 12
    여과filtered through activated alumina

실험 절차

Yellow 1-ethyl-3-methylimidazolium chloride (Aldrich) (50 g) was dissolved in deionized water (250 mL). Decolorizing charcoal (3 g) was added to the solution and the resulting mixture heated at 65° C. for 24 hours. The solution was cooled to room temperature and filtered. To the yellow filtrate was added decolorizing charcoal (3 g) and the solution was then heated for a further 24 hours at 65° C. The solution was allowed to cool to room temperature and then filtered to give a colorless solution. This solution was poured into a solution of lithium bis(trifluoromethanesulfonyl)amide (115 g) in 200 mL of deionized water. The solution was then stirred at room temperature for 3 hrs after which two layers had formed. The bottom layer was separated and washed three times with deionized water (100 mL). The layer was then heated at 65° C. under vacuum for 48 hrs and then filtered through activated alumina to give 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide as a colorless clean dry material in 87% yield.

출처