反应详情

A mixture of (S)-5-isopropyl-1-(3-(4-(1-((2-(trimethylsilyl)ethoxy)methyl)-1H-1,2,4-triazol-3-yl)phenyl)pyrazolo[1,5-a]pyrimidin-5-yl)imidazolidin-2-one (Example 25, Step 4, 12 mg, 0.023 mmol) and EtOH/6N aqueous HCl (1:2, 0.5 mL total) was heated at reflux for 3 hours. After cooling, the reaction mixture was neutralized by slow addition of saturated aqueous NaHCO3 solution. The mixture was extracted with dichloromethane, and the combined extracts were washed with brine, dried and concentrated. The residue was purified by column chromatography (12% MeOH in dichloromethane) to give (S)-1-(3-(4-(1H-1,2,4-triazol-3-yl)phenyl)pyrazolo[1,5-a]pyrimidin-5-yl)-5-isopropylimidazolidin-2-one (6 mg, 67%) as a pale yellow solid. LCMS (APCI+) m/z 389 [M+H]+.

1. temperaturewas heated
2. temperatureat reflux for 3 hours
3. temperatureAfter cooling
4. extractionThe mixture was extracted with dichloromethane
5. washthe combined extracts were washed with brine
6. customdried
7. concentrationconcentrated
8. customThe residue was purified by column chromatography (12% MeOH in dichloromethane)