2,3,3,3-Tetrafluoro-2-(trifluoromethyl)propanoyl fluoride → Potassium 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propanoate

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.

1. custom(equipped with a cold finger condenser, mechanical stirrer and a nitrogen inlet)
2. temperaturemaintained at -40°
3. temperaturethen it was cooled to -40°
4. stirringstirred overnight
5. filtrationThe solid was filtered under nitrogen
6. washwashed with dry ether
7. customdried under a stream of nitrogen

ORDレコード

ord-09bf57ad4f744b61bd86e8e655bf212e

出典データセット

uspto-grants-1988_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04723016