反应详情

温度

50 °C

A mixture of 3-{4-[(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-benzimidazol-2-yl)oxy]phenyl}-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (300 mg), 1 M TBAF in THF (6.3 mL), and TMEDA in THF (20 mL) was heated at 50° C. for 24 h. After cooling to rt, the mixture was partitioned between AcOEt and H2O. The organic layer was washed with brine, dried over Na2SO4 and evaporated. The residue was purified by column chromatography (SiO2, hexane/AcOEt=1/3 then AcOEt/MeOH=95/5). The obtained product was recrystallized from MeOH-iPr2O to give 3-[4-(1H-benzimidazol-2-yloxy)phenyl]-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (75 mg) as white crystals.

1. temperatureAfter cooling to rt
2. customthe mixture was partitioned between AcOEt and H2O
3. washThe organic layer was washed with brine
4. dry with materialdried over Na2SO4
5. customevaporated
6. customThe residue was purified by column chromatography (SiO2, hexane/AcOEt=1/3
7. customThe obtained product was recrystallized from MeOH-iPr2O