Methanol → HCID 23138126, compound

Participants

Reaction Steps

To a solution of N—(4-chlorophenyl)—N′—(2-hydroxy-2-methyl-1-((4-(5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)-1-piperazinyl)carbonyl)propyl)urea (0.18 g) obtained in Example 34 in dichloromethane (15 ml) was added trichloroacetyl isocyanate (0.065 ml) at 0° C., and the temperature of the mixture was elevated to room temperature and mixed at room temperature for 6 hours. To the reaction mixture were added methanol (5 ml), water (5 ml) and potassium carbonate (0.15 g), and then mixed at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, and then extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified with basic silica gel column (ethyl acetate to ethyl acetate/methanol=10/1) to obtain the title compound as colorless powder (0.12 g, 62%).

Provenance & Evidence