Water → HCID 12095352, compound

Participants

Reaction Conditions

Reaction Steps

0.28 g (15.5 mmol) of water is added to 14.04 g (19.3 mmol) of tris(nonafluorobutyl)difluorophosphorane, (C4F9)3PF2, 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. Liquid SO2 (about 5 ml), which is slowly released into the system, is via a T-piece connected in between with connected Young trap. The emulsion is stirred at 120° C. for 7.5 h before the intensive condenser is warmed to −5° C. in order to discharge excess SO2 in gaseous form. Virtually complete consumption (98.4%) of (C4F9)3PF2 and formation of (C4F9)3P═O (78.0%), (C4F9)2P(O)OH (14.0%) can be detected. The entire suspension is condensed at 75° C. in vacuo (10−3 mbar). Clear and colourless (C4F9)3P═O (8.81 g; 12.5 mmol; 79%) can be isolated in 92% purity. Pure, crystalline, clear and colourless (C4F9)2P(O)OH can be isolated from the solid residue by sublimation at 75° C. in vacuo (10−3 mbar).

Provenance & Evidence