Triphenylphosphine → 4-Chlorophenyldichlorophosphine

Participants

Reaction Steps

167 g (0.73 mole) of p-chlorophenylphosphonic acid dichloride and 121 g (0.46 mole) of triphenylphosphane were stirred for 2 hours at 180° C. and for 10 hours at 200° C. under an atmosphere of nitrogen. Distillation was then carried out at 0.04 kPa until a top temperature of 140° C. was reached. This gave 145 g, containing 58.5% of p-chlorophenyldichlorophosphane and 41.5% of p-chlorophenylphosphonic acid dichloride (according to 31P-NMR spectrum). The distillate was fractionated using a 70 cm silvered-jacketed column, packed with Raschig rings. Pure p-chlorophenyldichlorophosphane (boiling point: 71° C./0.093 kPa) was obtained. This corresponds to a yield of 85% of theory, based on triphenylphosphane employed.

Provenance & Evidence