Reaktion #319180

ord-6f027adf20ee499f9b8280bb33a85045

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAIT, and then at 100° for 4 hr
  2. 2
    SonstigeVolatile compounds were removed from the mixture under reduced pressure

Vorschrift

A mixture of 26.0 g (0.40 mole) of KCN, 150 ml of dimethyl formamide, 50 g (0.50 mole) of tetrafluoroethylene (TFE), and 50 g of CO2 was held at 50° for 4 hr., and then at 100° for 4 hr. at a maximum pressure of 1100 psi (7.6×103 kPa). The resulting mixture was dark and contained no insoluble salts. Volatile compounds were removed from the mixture under reduced pressure leaving a viscous residue of potassium 3-cyanotetrafluoropropionate, which substantially solidified to a deliquescent semisolid when triturated with ether. IR (neat): 2288 (weak covalently bound CN), 1680 (strong CO2), and 1250-1100 cm-1 (C--F, C--O) with broad H-bonded OH at 3450 and weak saturated CH at 2940 cm-1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04851161uspto-grants-1989_07