Triethylamine → HCID 14548451, compound

Participants

Reaction Steps

To a mixture of 17.0 g (4.31×10-2 mol) of 3,5-dicarbomethoxyphenyldiphenylphosphine oxide (from Preparation 3), 4.71 g (4.65×10-2 mol) of triethylamine and 196 ml of dry toluene under nitrogen was added 6.76 g (4.74×10-2 mol) of trichlorosilane. The mixture was then heated at reflux for 15.25 hr and cooled. A solution of 20% sodium hydroxide (49 ml) was added and the mixture was stirred. The organic layer was separated, washed with two 250 ml portions of water, dried over MgSO4 and concentrated to an oil which crystallized. The solid was recrystallized twice from methanol and dried. The yield of 3,5-dicarbomethoxyphenyldiphenylphosphine was 14.0 g (85.8% of theory); mp=103-4.5° C.

Provenance & Evidence