Tributylamine → 2,2'-Bis((diphenylphosphaneyl)methyl)-1,1'-binaphthalene

Participants

Reaction Steps

20.48 g (0.03 mol) of 2,2'-bis(diphenylphosphinylmethyl)-1,1'-binaphthyl are suspended in 80 ml of xylene and 30.6 g (0.165 mol) of tri-n-butylamine in the absence of air and moisture, and 26.57 g (0.15 mol) of phenyldichlorosilane are added dropwise with stirring. The mixture is then refluxed for 13 hours to give a clear solution. Xylene is distilled off at atmospheric pressure, and the mixture is allowed to cool with stirring. This results in the formation of 2,2'-bis(diphenylphosphinomethyl)-1,1'-binaphthyl as a colorless solid, which is filtered off under an inert gas and washed with 20 ml of degassed acetone. 18.5 g (95%) of colorless crystals of melting point 160° to 161° C. are obtained.

Provenance & Evidence