Trichloroacetic Acid → 81733-39-3

Participants

Reaction Steps

550 mg (2 mmol) of 4-hydroxycyclophosphamide and 210 mg (2 mmol) of ethylhydroxycarbamate (hydroxyurethane) are dissolved in 5 ml of dry methylenechloride free of alcohol. A catalytic amount of trichloroacetic acid and molecular sieve 4 A are added thereto. The reaction mixture is allowed to stand at -25° C. for 3 days. Thereafter, the molecular sieve is separated and washed once with a diluted solution of NaHCO3. The methylenechloride phase is dried over sodium sulfate and part of the solvent is evaporated in a vacuum and thereafter diluted with ether. After standing for 20 hours at -25° C., the separated crystals are filtered off, washed and dried.

Provenance & Evidence