تفاعل #1259160

ord-46c25535105848b285b5bc6c43c7e26d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was heated
  2. 2
    درجة الحرارةunder reflux for approximately 16 hours
  3. 3
    ترشيحThe reaction mixture was then filtered
  4. 4
    أخرىto remove the white KI precipitate
  5. 5
    أخرىformed
  6. 6
    أخرىthe filtrate was placed on a rotary evaporator for 4 hours
  7. 7
    أخرىto remove the acetone
  8. 8
    ترشيحThe oily liquid was then filtered a second time
  9. 9
    أخرىto yield the product

الإجراء التجريبي

1-Methylimidazole (4.32 g, 0.52 mol) was partially dissolved in reagent-grade toluene (50 ml) in a large round-bottomed flask and stirred vigorously. 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane (26 g, 0.053 mol) was added, and the mixture was heated under reflux at 110 degrees C. for 24 hours. The solvent was removed under vacuum giving 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide (30.5 g) as a waxy solid. Potassium 1,1,2,2-tetrafluoroethanesulfonate (TFES-K, 12 g) was added to reagent grade acetone (100 ml) in a separate round-bottomed flask, and this solution was carefully added to the 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide which had been dissolved in acetone (50 ml). The reaction mixture was heated under reflux for approximately 16 hours. The reaction mixture was then filtered using a large frit glass funnel to remove the white KI precipitate formed, and the filtrate was placed on a rotary evaporator for 4 hours to remove the acetone. The oily liquid was then filtered a second time to yield the product, as shown by proton NMR.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07829706B2uspto-grants-2010_11