Acetic Anhydride → HCID 53761108, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 47 g (0.55 mol) of cyanoacetic acid and 150 ml of acetic anhydride was added 73.1 g (0.51 mol) of 1-cyclopentyl-3-methylurea (XX). The solution was stirred at 70° C. for two hours. It was then evaporated and the residual oil (XXI) was dissolved in 400 ml of ethanol and 400 ml of water and 110 ml of 5 N NaOH was added in portions until the pH was over 7, under which the solution was boiled. It was then partly evaporated and crystals were filtered off. These crystals were a mixture of XX (~30%) and XXII (~70%) which was used for synthetizing XXII. Yield 30.8 g. NMR.

Provenance & Evidence