تفاعل #977757

ord-189c2bb10ac24f4eb6b1b87233954f89

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe biphasic mixture stirred at room temperature for 20 h
  2. 2
    أخرىthe layers separated
  3. 3
    غسيلThe organic layer was washed with water (3×75 mL) until the washings
  4. 4
    أخرىAfter drying
  5. 5
    أخرى(MgSO4), removal of the solvent in vacuum
  6. 6
    أخرىgave a viscous gum which
  7. 7
    أخرىwas further dried

الإجراء التجريبي

To a suspension of perfluorooctanesulfonic acid potassium salt (10.76 g, 20.0 mmol) in water (100 mL) at room temperature under nitrogen was added dropwise triphenylsulfonium bromide (6.87 g, 20.0 mmol) over 15 min. After stirring the suspension for 30 min., dichloromethane (100 mL) was added and the biphasic mixture stirred at room temperature for 20 h. Additional dichloromethane (100 mL) was added and the layers separated. The organic layer was washed with water (3×75 mL) until the washings were neutral (pH 7). After drying (MgSO4), removal of the solvent in vacuum gave a viscous gum which was further dried by heating at 50° C. for 24 h under vacuum. In this way, triphenylsulfonium perfluorooctanesulfonate was isolated as a pale yellow gummy solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: USRE038980E1uspto-grants-2006_02