Phosphorus trichloride → Phosphorimidic trichloride, (trimethylsilyl)-

Participants

Reaction Steps

Diethyl ether (250 ml) was added with stirring to a flask cooled in an ice/water bath containing lithium bis(trimethylsilyl)amide (27.7 g, 0.17 mol). Phosphorus trichloride (14.5 ml, 0.17 mol) was then added and the mixture stirred for a further 5-10 minutes before removing the ice water bath. Stirring was continued at ambient temperature for a further 1-2 hours. The reaction flask was then cooled again in an ice/water bath and sulfuryl chloride (13.3 ml, 0.17 mol) added. The mixture was stirred for a further 10-15 minutes before removing the ice/water bath and stirring at ambient for a further 1-2 hours or until the reaction was complete, as indicated by 31P {1H} NMR spectroscopy. The product was isolated in pure form via vacuum distillation.

Provenance & Evidence