反应详情

温度

60 °C

To a solution of 1-(2-cyclopropyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one (100 mg), (4-chloro-3-fluorophenyl)methanol (114 mg) and tributylphosphine (258 μl) in THF (15 ml) was added 1,1′-(azodicarbonyl)dipiperidine (265 mg). The mixture was stirred under sonication at 60° C. for 2 h. The reaction mixture was then cooled to room temperature, and concentrated in vacuo. The residue was diluted with DCM, washed with water and brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH/DCM) to give the title compound (25 mg) as an off-white solid.

1. temperatureThe reaction mixture was then cooled to room temperature
2. concentrationconcentrated in vacuo
3. additionThe residue was diluted with DCM
4. washwashed with water and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by silica gel column chromatography (MeOH/DCM)