反应详情

温度

60 °C

To a solution of 1-(2-ethyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one (150 mg), (5-chloro-2-thienyl) methanol (166 mg) and tributylphosphine (388 mg) in THF (10 ml) was added 1,1′-(azodicarbonyl)dipiperidine (422 mg), and the reaction mixture was stirred at 60° C. for 2 h. The reaction mixture was cooled to room temperature. The mixture was poured into water and extracted with EtOAc. The extract was washed with brine, dried over MgSO4, concentrated and purified by NH silica gel column chromatography (hexane/EtOAc then EtOAc/MeOH). The resulting solid was recrystallized from EtOH-hexane to give the title compound (16.1 mg) as a white solid.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionextracted with EtOAc
3. washThe extract was washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. custompurified by NH silica gel column chromatography (hexane/EtOAc
7. customThe resulting solid was recrystallized from EtOH-hexane