Реакция #2444878

ord-d791c06bcbb740e2be499f2c45814870

Растворители

Условия реакции

Температура
65°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe solution was cooled to room temperature
  2. 2
    Фильтрацияfiltered
  3. 3
    workup.ADDITIONTo the yellow filtrate was added
  4. 4
    Температураthe solution was then heated for a further 24 hours at 65° C
  5. 5
    Температураto cool to room temperature
  6. 6
    Фильтрацияfiltered
  7. 7
    Другоеto give a colorless solution
  8. 8
    Другоеhad formed
  9. 9
    ДругоеThe bottom layer was separated
  10. 10
    Промывкаwashed three times with deionized water (100 mL)
  11. 11
    ТемператураThe layer was then heated at 65° C. under vacuum for 48 hrs
  12. 12
    Фильтрацияfiltered through activated alumina

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07763186B2uspto-grants-2010_07