Reacción #4042

ord-09bf57ad4f744b61bd86e8e655bf212e

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otro(equipped with a cold finger condenser, mechanical stirrer and a nitrogen inlet)
  2. 2
    Temperaturamaintained at -40°
  3. 3
    Temperaturathen it was cooled to -40°
  4. 4
    workup.STIRRINGstirred overnight
  5. 5
    FiltraciónThe solid was filtered under nitrogen
  6. 6
    Lavadowashed with dry ether
  7. 7
    Otrodried under a stream of nitrogen

Procedimiento

Perfluoroisobutyryl fluoride (17.76 g, 82 mmol) was distilled into a 3-neck flask (equipped with a cold finger condenser, mechanical stirrer and a nitrogen inlet) containing a slurry of potassium trimethylsilanolate (10.26 g, 80 mmol) in dry ether (500 mL). The mixture was stirred 3 h at room temperature with the condenser maintained at -40°; then it was cooled to -40° and stirred overnight. The solid was filtered under nitrogen, washed with dry ether, and dried under a stream of nitrogen to afford potassium perfluoroisobutyrate (12.29 g, 61% yield) as a white solid: 19F NMR (D2O) δ -72.2 (d, J=7.5 Hz, CF3, 6F), -171.8 ppm (sp, J=7.5 Hz, CF, 1F). Anal. Calcd. for C4F7KO2 : C, 19.05; F, 52.75. Found: C, 19.12; F, 52.70.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04723016uspto-grants-1988_02