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 (150 mg), 4-chlorothiophen-2-methanol (158 mg) and tributylphosphine (322 mg) in THF (15 ml) was added 1,1′-(azodicarbonyl)dipiperidine (401 mg). The mixture was stirred at 60° C. for 4 h. The reaction mixture was concentrated in vacuo, and diluted with DCM. The organic layer 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 (53 mg) as an off-white solid.

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