تفاعل #53247

ord-71bd1248fad64cd58c8f6ed57ff96111

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىa solution obtained
  2. 2
    workup.ADDITIONwas added to the above solution
  3. 3
    استخلاصThe aqueous solution was extracted twice with 100 ml of chloroform
  4. 4
    غسيلthe organic phase was washed with water
  5. 5
    تركيزconcentrated
  6. 6
    أخرىan oily product was obtained
  7. 7
    تركيزThe above-obtained product was concentrated again with ethyl acetate
  8. 8
    أخرىa solid product was obtained
  9. 9
    ترشيحThe solid product was filtered and re-slurried with diisopropyl ether

الإجراء التجريبي

Potassium perfluorobutanesulfonate (10 g) was dissolved in a mixed solvent comprising 500 ml of water and 100 ml of methanol, and a solution obtained by dissolving 7.7 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide in 50 ml of methanol was added to the above solution. The aqueous solution was extracted twice with 100 ml of chloroform, the organic phase was washed with water and concentrated, thereby an oily product was obtained. The above-obtained product was concentrated again with ethyl acetate, thereby a solid product was obtained. The solid product was filtered and re-slurried with diisopropyl ether, to thereby obtain 9 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858370B2uspto-grants-2005_02