Trichloroacetic Acid → 2-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-3-yl-thio]-ethanesulphonic acid ammonium salt

Participants

Reaction Steps

2.8 g (10 mmol), of 4-hydroxycyclophosphamide and 1.6 g (10 mmol) of ammonium-2-mercaptoethanesulphonate were dissolved with a cataytic quantity of trichloroacetic acid in 10 ml of dimethylformamide and were stored in a refrigerator at -25° C. for 20 hours. After a further 5 hours at 0° C., the mixture was mixed with ehter until clouding commenced and was triturbated. The crystrallised material was filtered with suction after 1 day at 0° C., washed dried and recrystallised from n-propanol.

Provenance & Evidence