تفاعل #53243

ord-19f779f8d65149fe8fe5ea29e4bab2a9

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
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 200 ml of chloroform
  4. 4
    غسيلthe organic phase was washed with water
  5. 5
    تركيزconcentrated
  6. 6
    أخرىa crude product was obtained
  7. 7
    درجة الحرارةcooling
  8. 8
    أخرىa solid product was precipitated
  9. 9
    ترشيحThe precipitate was filtered and re-slurried with diisopropyl ether

الإجراء التجريبي

Potassium perfluorobutanesulfonate (60 g) was dissolved in a mixed solvent comprising 200 ml of water and 200 ml of methanol, and a solution obtained by dissolving 49.5 g of phenacyltetrahydrothiophenium bromide in 300 ml of water was added to the above solution. The aqueous solution was extracted twice with 200 ml of chloroform, the organic phase was washed with water and concentrated, thereby a crude product was obtained. Distilled water (300 ml) was added to the above-obtained product, followed by heating at 100° C. for 30 minutes and then cooling, thereby a solid product was precipitated. The precipitate was filtered and re-slurried with diisopropyl ether, thereby 77 g of phenacyltetrahydrothiophenium perfluorobutanesulfonate was obtained.

المصدر

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