反应详情

温度

60 °C

To a solution of 1-(2-cyclopropyl-1-methyl-1H-benzimidazol-6-yl)-4-(hydroxymethyl)pyridin-2(1H)-one (150 mg), 4-chlorophenol (130 mg) and tributylphosphine (514 mg) in THF (15 ml) was added 1,1′-(azodicarbonyl)dipiperidine (641 mg), and the mixture was stirred at 60° C. for 4 h. The mixture was concentrated in vacuo, and diluted with DCM. The mixture was washed with water and brine successively, dried over Na2SO4, concentrated in vacuo and purified by column chromatography (MeOH/DCM) to afford the title compound (45 mg) as a white solid.

1. concentrationThe mixture was concentrated in vacuo
2. additiondiluted with DCM
3. washThe mixture was washed with water and brine successively
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. custompurified by column chromatography (MeOH/DCM)