Triethyl phosphite → HCID 178436118, compound

Participants

Reaction Steps

Vinyl benzene phosphonate was prepared by chloromethylating benzene by the procedure of Kindler, Hansen and Koebk (Ann. Chem. 617, 25, 1958). 1 mole p-(2-chloroethyl)-α-chlorotoluene was heated to 140°-155° C. under N2 and 95 ml triethyl phosphite was added. The mixture was heated for one hour and then diethyl-p-(2-chloroethyl)-benzyl phosphonate was distilled off at 140°-150° C./0.2 torr. The ethyl ester was hydrolysed for two hours using a 2:3 v/v mixture of 48% HBr and formic acid. The product was dehydrochlorinated using potassium ethoxide followed by acidification with HCl. The monomer was then flash distilled using 10-5 torr vacuum at room temperature.

Provenance & Evidence