Nitrogen → HCID 86737607, compound

Participants

Reaction Steps

200 g of phosgene were passed into 1 mole of propane-phosphonic acid diethyl ester at 70°-80° C. The mixture was stirred at 70°-80° C. for 1 hour and a dry N2 stream was passed through the reaction mixture overnight at 50° C. The mixture was completely degassed at 50° C. under a waterpump vacuum in a Rotavapor and crude propanephosphonic acid ethyl ester-chloride was obtained. This was rendered basic with absolute pyridine, dissolved in 300 ml of toluene and reacted with a mixture of 1.1 moles of pyridine and 1 mole of allyl alcohol at 20°-30° C. The mixture was allowed to after-react at 80° C. for 2 hours. The solution which was separated off from the hydrochloride by filtration was concentrated and distilled.

Provenance & Evidence