反应详情

温度

200 °C

The mixture of 1-ethyl-3-(4-hydroxyphenyl)-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (281 mg), 2-(methylsulfonyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazo[4,5-b]pyridine (240 mg) and NaH (35.2 mg) in DMF(dry) (3 mL) was heated at 200° C. for 3 h under microwave irradiation. The reaction mixture was diluted with MeOH, and concentrated in vacuo. The residue was diluted with 6N HCl. The mixture was neutralized with aq. NaHCO3 at 0° C. and extracted with EtOAc. The organic layer was separated, washed with water and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography (silica gel, eluted with 0%-100% EtOAc in hexane) to give 1-ethyl-3-[4-(3H-imidazo[4,5-b]pyridin-2-yloxy)phenyl]-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (40 mg) as white crystals.

1. concentrationconcentrated in vacuo
2. additionThe residue was diluted with 6N HCl
3. customwas neutralized with aq. NaHCO3 at 0° C.
4. extractionextracted with EtOAc
5. customThe organic layer was separated
6. washwashed with water and brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo
9. customThe residue was purified by column chromatography (silica gel, eluted with 0%-100% EtOAc in hexane)