66197-72-6

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: (according to P. C. Crofts, G. M. Kosolapoff J. Am. Chem. Soc. 1953, 75, 5738-40) 126 g of triethyl phosphite and 162 g of dibromomethane are heated to 170° C. in an autoclave for 4 hours. Bromomethylphosphonic acid diethyl ester may be isolated in moderate yield from the reaction mixture by distillation (b.p.: approx. 50° C., 7 Pa (0.05 Torr)). A second fractional distillation was then performed.