Water → 4-Acetyl-2,3,4,5-tetrahydro-1H-1,4-benzodiazepine-1-carboxamide

Participants

Reaction Conditions

Reaction Steps

To a solution of 4-acetylbenzodiazepine (20.0 g, 0.105 mole) in acetonitrile (100 ml) at room temperature was added sodium cyanate (27.4 g, 0.42 mole). The resulting suspension was heated to 50° C. and then trifluoroacetic acid (24.0 g, 0.21 mole) was added slowly dropwise over 30 min. Heating was continued at 50° C. for 1 h. The reaction mixture was cooled to room temperature and the solvent was evaporated to give a white residue. Water (160 ml) was added to the residue and the mixture was cooled in ice for 1 h. The solids were collected by filtration and washed with cold water. After drying under house vacuum 23.6 g (96% ) of product was obtained as a white solid.

Provenance & Evidence