“…The remaining solution was concentrated on a rotary evaporator, without heating'O, and the resultant oil was chromatographed on a column (2.2 cm X 25 cm) of silica gel using ethyl acetate as the eluent. Compound IV (Rf 0.5, ethyl acetate) was eluted with 85-135 ml of solvent and was obtained as a pale-yellow oil (252 mg, 20% yield); 31P-NMR (deuterium oxide): 6 3-Chlorocyclophosphamide (V)-A magnetically stirred solution of IeH20 (270 mg, 0.97 mmole) in chloroform (15 ml) was cooled with an ice-water bath, and an aqueous solution of sodium hypochlorite" [15 ml, 5.25% (w/w) NaOCI, 10.6 mmoles] was added; after 4 hr, the water bath was removed. Aliquots (1 ml) of the chloroform layer were periodically removed, diluted with deuterochloroform (1 ml), and the relative signal intensities for I(612.10) and the only detectable product (615.95) were measured by "P-NMR 5050.…”