反应详情

To a stirred suspension of NaH (40% oil dispersion, 50 mg) in THF (9 ml) was added a solution of 1-(2-cyclopropyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one (150 mg) in THF (1 ml) at 0° C., and then the mixture was stirred at room temperature for 30 min. 1-Bromomethyl-2-fluorobenzene (150 mg) in THF (0.5 ml) was added, and the resulting mixture was stirred at room temperature for 12 h. The reaction mixture was quenched with ice-water and extracted with DCM. The extract was washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by silica gel column chromatography (MeOH/DCM) followed by crystallization with DCM/hexane (19:1, 2 ml) to give the title compound (56 mg) as a white solid.

1. stirringthe resulting mixture was stirred at room temperature for 12 h
2. customThe reaction mixture was quenched with ice-water
3. extractionextracted with DCM
4. washThe extract was washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by silica gel column chromatography (MeOH/DCM)
8. customfollowed by crystallization with DCM/hexane (19:1, 2 ml)