601139 Disclosed is a method for the preparation of a compound of formula (D) (isophosphoramide mustard, IPM) comprising treating a benzyl isophosphoramide compound of formula (C) with a reducing agent under hydrogenolysis conditions, wherein as valence and stability permit, X and Y independently represent leaving groups and R1 is benzyl optionally substituted with one or more substituents selected from halogen, R2, OR2 and NR22 wherein R2 is selected in each occurrence from H and lower alkyl wherein the hydrogenolysis conditions comprise hydrogen gas with a pressure greater than 1 atm.