反应详情

To tert-butyl 1-((4-(5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)-1-piperidinyl)carbonyl)pentylcarbamate (0.65 g) obtained in Example 80b) was added concentrated hydrochloric acid (5 ml), and mixed for 15 minutes. To the reaction solution was added ethanol, and then concentrated under reduced pressure. The residue and DBU (0.69 g) were dissolved in acetonitrile (15 ml), and a solution of 4-chlorophenyl isocyanate (0.25 g) in acetonitrile (15 ml) was added dropwise thereto. After reacting for 15 hours, the solvent was distilled off under reduced pressure, and the residue was purified with silica gel column (ethyl acetate to ethyl acetate/methanol=5/1). The product was recrystallized from ethyl acetate-diisopropyl ether to obtain the title compound as colorless powder (0.37 g, 51%).

1. additionmixed for 15 minutes
2. concentrationconcentrated under reduced pressure
3. dissolutionThe residue and DBU (0.69 g) were dissolved in acetonitrile (15 ml)
4. additiona solution of 4-chlorophenyl isocyanate (0.25 g) in acetonitrile (15 ml) was added dropwise
5. distillationthe solvent was distilled off under reduced pressure
6. customthe residue was purified with silica gel column (ethyl acetate to ethyl acetate/methanol=5/1)
7. customThe product was recrystallized from ethyl acetate-diisopropyl ether