反应详情

温度

20 °C

0.30 g (16.7 mmol) of water and 3.19 g (53.1 mmol) of fire-extinguishing sand as SiO2 source are added to 12.0 g (28.0 mmol) of tris(pentafluoroethyl)difluorophosphorane, (C2F5)3PF2, in a 100 ml glass round-bottomed flask and warmed (20° C. oil-bath temperature). An intensive reflux condenser is connected downstream of the flask. The suspension is stirred at 120° C. for 4 h. Complete consumption of (C2F5)3PF2 and formation of (C2F5)3P═O (72.0%) and (C2F5)2P(O)OH (28.0%) can be detected. The entire suspension is condensed at room temperature in vacuo (10−3 mbar). Clear and colourless (C2F5)3P═O (6.27 g; 15.5 mmol; 55%) can be isolated in 99% purity. Further (C2F5)3P═O can be isolated from the solid residue by extraction.

1. customAn intensive reflux condenser is connected
2. customconsumption of (C2F5)3PF2 and formation of (C2F5)3P═O (72.0%) and (C2F5)2P(O)OH (28.0%)
3. customcondensed at room temperature in vacuo (10−3 mbar)