反应详情

温度

60 °C

To a mixture of 1-(2-ethyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one (126 mg), (5-chloro-3-thienyl)methanol (139 mg) and tributylphosphine (0.347 ml) in THF (8 ml) was added 1,1′-(azodicarbonyl)dipiperidine (354 mg), and the mixture was stirred at 60° C. for 2 h. The reaction mixture was partitioned between EtOAc and water, and the organic layer was washed with brine, dried MgSO4, and concentrated in vacuo. The residue was purified by NH silica gel column chromatography (hexane/EtOAc to MeOH/EtOAc). The resulting solid was recrystallized from EtOH/hexane to give the title compound (90 mg) as a white solid.

1. customThe reaction mixture was partitioned between EtOAc and water
2. washthe organic layer was washed with brine, dried MgSO4
3. concentrationconcentrated in vacuo
4. customThe residue was purified by NH silica gel column chromatography (hexane/EtOAc to MeOH/EtOAc)
5. customThe resulting solid was recrystallized from EtOH/hexane