反应详情

To a solution of 0.085 g (0.49 mmol) of 5,7-dimethyl-2-ethylimidazo[4,5-b]pyridine in 1.0 mL anhydrous DMF was added 21.0 mg (0.54 mmol) of a 60% oil dispersion of sodium hydride and the reaction mixture was stirred under a nitrogen atmosphere at room temperature for 1 hour. A solution of 0.250 g (0.56 mmol) of the product of Step C in 0.5 mL of DMF was added and the reaction was stirred an additional 2 hours at room temperature. The reaction mixture was partitioned between EtOAc and water, separated, dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 50% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded 0.150 g (58%) of the title compound.

1. stirringthe reaction was stirred an additional 2 hours at room temperature
2. customThe reaction mixture was partitioned between EtOAc and water
3. customseparated
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified on a silica gel flash chromatography column
8. washeluted with 50% EtOAc-hexane
9. customEvaporation of the purified fractions
10. customdrying in vacuo