反应详情

750 mg (2.7 mmol) of 4-hydroxycyclophosphamide and 450 mg (2.7 mmol) of benzyl-hydroxycarbamate are dissolved in 6 ml of methylene chloride free of alcohol. A small amount of trichloroacetic acid is added thereto and the solution is allowed to stand at -25° C. in a refrigerator for 3 days. The resulting solution is filtered off, the mother liquor is diluted with 5 ml of chloroform, then is diluted with water and thereafter is washed with a dilute solution of NaHCO3 and with water. The washed solution is dried over sodium sulfate and is evaporated in a vacuum. The oily residue thereafter is recrystallized from acetic acid ethyl ester containing a small amount of methanol.

1. filtrationThe resulting solution is filtered off
2. additionthe mother liquor is diluted with 5 ml of chloroform
3. additionis diluted with water
4. washis washed with a dilute solution of NaHCO3 and with water
5. dry with materialThe washed solution is dried over sodium sulfate
6. customis evaporated in a vacuum
7. customThe oily residue thereafter is recrystallized from acetic acid ethyl ester containing a small amount of methanol