反应详情

温度

50 °C

1-[(2,2-Difluorocyclopropyl)methyl]-5-[2-(4-methoxyphenyl)-2-azabicyclo-[2.2.2]oct-5-en-5-yl]-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (6-2, 52 mg, 0.12 mmol, 1.0 equiv) was added to CH3CN (1 mL) and water (1 mL). To this suspension was added aqueous H2SO4 (115 μL, 0.12 mmol, 1.0 equiv, 1.0 M) followed by periodic acid in one portion (26 mg, 0.12 mmol, 1.0 equiv). The reaction contents were heated to 50° C. for 18 h. Following this duration, LCMS showed consumption of starting material. The mixture was subsequently filtered through Celite, rinsed with CH3CN and purified by reverse-phase HPLC (10-90% CH3CN:H2O) to give 6-3 as an off-white solid. MS m/z (M+H): calculated=346.4; observed=347.1.

1. customThe reaction contents
2. customconsumption of starting material
3. filtrationThe mixture was subsequently filtered through Celite
4. washrinsed with CH3CN
5. custompurified by reverse-phase HPLC (10-90% CH3CN:H2O)