Triethylamine → HCID 67026219, compound

Participants

Reaction Steps

Into a 1 L Schlenk flask was added the phosphine oxide (3a) (17.21 g, 66.7 mmol). To this was added acetonitrile (400 ml) and triethylamine (27.9 ml, 200.1 mmol). Then trichlorosilane (20.2 ml, 200.1 mmol) was added slowly. The addition of the trichlorosilane gave the formation of some white precipitate. The resultant mixture was then refluxed overnight. The resultant suspension was then cooled to 0° in an ice bath and a solution of potassium hydroxide (40 g) in water (200 ml) which had been degassed with nitrogen gas was added slowly. This gave a bi-phasic mixture. Additional acetonitrile (100 ml) was then added. The upper organic phase was then removed by cannula into a clean Schlenk flask and the solvent removed under vacuum. This gave an off-white solid (3b). Yield=13.60 g, 84%.

Provenance & Evidence