反应详情

温度

120 °C

12.01 g (28.0 mmol) of tris(pentafluoroethyl)difluorophosphorane, (C2F5)3PF2, are initially introduced in a 100 ml glass round-bottomed flask and warmed (120° C. oil-bath temperature). A cooled (−30° C. to −35° C.) intensive reflux condenser is connected downstream of the flask. A 250 ml glass round-bottomed flask containing dry ice is connected via a T-piece so that gaseous CO2 is forced through the phosphorane liquid. The liquid is stirred at 120° C. for 6 h. In this time, a total of about 400 g (9 mol) of CO2 are bubbled through the hot liquid. After 6 h, the condenser temperature is warmed to −5° C. The clear and colourless liquid remaining (4.53 g) consists of (C2F5)3PF2 (49%), (C2F5)3P═O (49%) and (C2F5)2P(O)OH (2%). Tris(pentafluoroethyl)phosphine oxide, (C2F5)3P═O, is isolated from the reaction mixture by distillation.

1. temperatureA cooled (−30° C. to −35° C.) intensive reflux condenser
2. waitAfter 6 h
3. temperaturethe condenser temperature is warmed to −5° C