Reaktion #4031

Reaktionsgleichung

Methyl perfluorobutyrate

sodium trimethylsilanolate

→

sodium perfluorobutyrate

Ausbeute 84.0%

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe solid was filtered under nitrogen
2. 2
   Waschenwashed with dry ether
3. 3
   Sonstigedried under a stream of nitrogen

Vorschrift

Methyl perfluorobutyrate (12.81 g, 56 mmol) was added dropwise to a stirred solution of sodium trimethylsilanolate (6.3 g, 56 mmol) in dry ether (300 mL) at room temperature under nitrogen. The reaction mixture was stirred overnight. The solid was filtered under nitrogen, washed with dry ether, and dried under a stream of nitrogen to afford sodium perfluorobutyrate (11.1 g, 84% yield) as a white solid: 19F NMR (D2O) δ -79.6 (t, J=8 Hz, CF3 --, 3F), -117.2 (q, J=8 Hz, CF3CF2CF2 --, 2F), -126.2 ppm (s, CF3CF2 --, 2F). Anal. Calcd. for C4F7NaO2 : C, 20.36; F, 56.35; Na, 9.74. Found: C, 20.84, 20.61, 20.58; F, 56.68, 53.24; Na, 9.89, 9.65.

Quelle