反应详情

To a solution of 0.020 g (0.10 mmol) of 1-carboethoxy-2-benzimidazolinone dissolved in 250 gL DMF was added 0.035 g (0.11 mmol) of cesium carbonate and the resulting suspension was stirred under a nitrogen atmosphere for 10 minutes. A solution of the product of step B in 300 aL DMF was then added and the reaction mixture was stirred for an additional 1 hour. The mixture was suspended in 10% aqueous citric acid and extracted into ethyl acetate. The organic layer was separated, washed with saturated sodium bicarbonate and brine, dried (MgSO4), filtered, 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 0.029 g (58%) of the title compound.

1. stirringthe reaction mixture was stirred for an additional 1 hour
2. extractionextracted into ethyl acetate
3. customThe organic layer was separated
4. washwashed with saturated sodium bicarbonate and brine
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