Ammonia → Ethyl diphenylphosphinite

Participants

Reaction Steps

1000 g (21.7 mol) of absolute ethanol are cooled to -15° C. with stirring under a nitrogen atmosphere. 660 g (3.0 mol) of chloro(diphenyl)phosphine are then added dropwise at this temperature with vigorous stirring in the course of one hour and twenty minutes. 76 g (4.47 mol) of ammonia gas are then introduced at this temperature with further vigorous stirring. The mixture is then allowed to come to room temperature with stirring and is stirred for a further six hours. The mixture is then filtered with suction and rinsed out with ethanol. The filtrate is freed from ethanol and excess ammonia in vacuo. A crude product is obtained which is freed from a slight salt precipitate by filtration through a glass 5 frit. 635 g of ethyl diphenylphosphinite are obtained by thin film distillation at a bath temperature of 160° to 175° C. and a pressure of about 0.5 mbar. This corresponds to a yield of 92% of theory.

Provenance & Evidence