Reaktion #1483137

ord-abef295c47084e70a76e02e0c35b889b

Reaktionsgleichung

O=S(=O)([O-])C(F)(F)C(F)(F)CCO.[Na+]
sodium 4-hydroxy-1,1,2,2-tetrafluorobutane-1-sulfonate
OCCC(F)(F)C(F)(F)Br
4-bromo-3,3,4,4-tetrafluoro-1-butanol
O=S(=O)(O)C(F)(F)C(F)(F)CCO
4-Hydroxy-1,1,2,2-tetrafluorobutane-1-sulfonic acid

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionwas extracted with methanol (100 mL)
  2. 2
    Filtrationfiltered
  3. 3
    Sonstigeto give a light brown solution
  4. 4
    Sonstigeto flush any remaining sulfonic acid
  5. 5
    SonstigeThe volatiles were removed under reduced pressure
  6. 6
    Sonstigeto give a dark brown oil

Vorschrift

The solid from above which contained sodium 4-hydroxy-1,1,2,2-tetrafluorobutane-1-sulfonate was extracted with methanol (100 mL) and filtered. The resulting pale yellow solution was passed through a short column (2.5 cm diameter) which was packed with 7.5 cm of Amberlite 120H acid ion exchange resin to give a light brown solution. Additional methanol was used to flush any remaining sulfonic acid. The volatiles were removed under reduced pressure to give a dark brown oil. The yield was 15.453 g, 77% based on starting 4-bromo-3,3,4,4-tetrafluoro-1-butanol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08900792B2uspto-grants-2014_12