Acetic Acid → N-(2-cyano-3-methylbutanoyl)urea

Participants

Reaction Steps

Cyanoacetylurea (25.8 g) was suspended in acetone (258 ml), and acetic acid (2.4 g) and ammonium acetate (1.5 g) were added. This suspension was subjected to catalytic hydrogenation in the presence of 5% palladium carbon (2.1 g, 50% wet product) under hydrogen pressure at 10 kg/cm2 and at 40° C. for 1 hour. The reaction mixture was refluxed under heating to dissolve an insoluble matter, and the catalyst was filtered off. The obtained filtrate was concentrated to a half. Water (130 ml) was added to the filtrate to allow precipitation of crystals. The crystals were collected by filtration to give crystals of N-(2-cyano-3-methylbutanoyl)urea (yield 30.7 g).

Provenance & Evidence