反应详情

Ethoxycarbonyl isothiocyanate (0.096 mL, 0.85 mmol) was added to 4-{[(6-phenoxypyridin-3-yl)methyl]amino}-1H-imidazole-5-carboxamide (0.25 g, 0.81 mmol, obtained from Example 25(a)) in anhydrous dichloromethane (3.0 mL). After stirring for 2.5 h at ambient temperature the mixture was concentrated to dryness. Sodium hydroxide (10 mL, 2% w/v) was added and the solution was heated at 50° C. over night. After cooling, the pH was adjusted to 4-5 using 2N HCl. The solid was collected by filtration and recrystallized from DMSO/water to give a white crystalline material. A portion of this material was recrystallized from MeOH to give 35 mg (0.10 mmol, 12% yield) of the title compound.

1. concentrationwas concentrated to dryness
2. additionSodium hydroxide (10 mL, 2% w/v) was added
3. temperaturethe solution was heated at 50° C. over night
4. temperatureAfter cooling
5. filtrationThe solid was collected by filtration
6. customrecrystallized from DMSO/water
7. customto give a white crystalline material
8. customA portion of this material was recrystallized from MeOH