反应详情

To a solution of 0.069 g (0.33 mmol) of 1-carboethoxy-2-benzimidazolinone dissolved in 0.6 mL DMF was added 0.217 g (0.66 mmol) of powdered cesium carbonate and the resulting suspension was stirred under a nitrogen atmosphere at room temperature for 30 minutes. A solution of the product of step E in 0.5 mL DMF was then added and the reaction mixture was stirred for an additional 15 hours. The mixture was then partitioned between EtOAc and water and extracted. The organic layer was separated, dried (MgSO4), filtered and evaporated, and the residue was purified on a silica gel flash chromatography column eluted with 30% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded 0.088 g (45%) of the title compound.

1. stirringthe reaction mixture was stirred for an additional 15 hours
2. customThe mixture was then partitioned between EtOAc and water
3. extractionextracted
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customthe residue was purified on a silica gel flash chromatography column
9. washeluted with 30% EtOAc-hexane
10. customEvaporation of the purified fractions
11. customdrying in vacuo