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 (224 mg), (5-fluorothiophen-2-yl)methanol (100 mg) and tributylphosphine (750 mg) in THF (15 ml) was added 1,1′-(azodicarbonyl)dipiperidine (956 mg), and the mixture was stirred at 60° C. for 4 h. The reaction 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 silica gel column chromatography (MeOH/DCM) followed by preparative HPLC to afford the title compound (20 mg) as a white solid.

1. concentrationThe reaction 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 silica gel column chromatography (MeOH/DCM)