反应详情

To a solution of 0.120 g (0.62 mmol) of 3,5-dichloro-4-hydroxybenzyl alcohol in 1.5 mL DMF was added 0.223 g (0.68 mmol) of cesium carbonate and the reaction was magnetically stirred at room temperature for 15 minutes. A solution of 0.196 g (0.68 mmol) of ethyl α-bromo-3,4-methylenedioxyphenylacetate in 0.5 mL DMF was added and the reaction was stirred an additional 30 minutes at room temperature. The reaction mixture was partitioned between EtOAc and 5% aqueous citric acid, extracted, dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 30% EtOAc-hexane, and evaporation of the purified fractions afforded 0.214 g (86%) of the title compound.

1. stirringthe reaction was stirred an additional 30 minutes at room temperature
2. customThe reaction mixture was partitioned between EtOAc and 5% aqueous citric acid
3. extractionextracted
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified on a silica gel flash chromatography column
8. washeluted with 30% EtOAc-hexane, and evaporation of the purified fractions