Hydrochloric Acid → Tributylphosphine oxide

Participants

Reaction Steps

116.5 g (1 mol) chlorosulfonic acid was placed in an apparatus as described in Example 4 and reacted therein within 60 minutes with 208 g (1 mol) tributylphosphane at 18°-20° C. while cooling with ice. Towards the end of the reaction when cooling was stopped, the reaction temperature rose to 34° C. The whole was stripped at 70° C. under a pressure of 0.5 millibar. This was accompanied by a violent exothermal reaction. The temperature rose up to 140° C. The material was stripped once again at 80° C. under a pressure of 1 millibar. 263 g tributylphosphane oxide was obtained in the form of a HCl-adduct (determined by elementary analysis and 31P -NMR-spectroscopy). 90% P was in the form of a tributylphosphane oxide HCl-adduct.

Provenance & Evidence