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 (127 mg), (5-fluorothiophen-2-yl)methanol (40 mg) and tributylphosphine (182 mg) in THF (15 ml) was added 1,1′-(azodicarbonyl)dipiperidine (227 mg), and the mixture was stirred at 60° C. for 4 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 successively, dried over Na2SO4, concentrated in vacuo and purified by column chromatography (MeOH/DCM) followed by preparative HPLC to afford the title compound (6 mg) as a 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 successively
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. custompurified by column chromatography (MeOH/DCM)