Mitarson,Asta-Werke,W. Germany,1961
A solution of 8 g of ethylene chlorohydrin and 10.2 g of triethylamine in 50 cc
of absolute dioxane is slowly added dropwise to a solution of 25.9 g of N,Nbis-(β-chloroethyl)-phosphoric acid amide dichloride in 100 cc of absolute
dioxane. The mixture is then heated for 2 hours at 60°C. After cooling, a
solution of 7.5 g of 1,3-propanolamine and 10.2 g of triethylamine in 50 cc of
absolute dioxane is added dropwise while stirring well and at a temperature
up to 30°C. The mixture is left to stand for another 12 hours. The liquid is
filtered off with suction from the precipitated triethyamine hydrochloride. The
filtrate is filtered through carbon and concentrated by evaporation in water-jet
vacuum at 40°C. The residue is dissolved in a little alcohol. Copious amounts of ether are added and the solution is left overnight in a refrigerator. It is then
again filtered through carbon, the ether is evaporated and the residual volatile
fractions are removed under high vacuum at 55°C. The result is a yellowish,
fairly viscous oil, which is insoluble in water.
