反应详情

3.0 g of sodium hydrogen carbonate was suspended in 90 mL DMF. At 0° C. a solution of 5.15 g of 4-nitrocatechol was added dropwise over 15 min. Subsequently, 3.9 g of epichlorohydrin in 10 mL DMF were added over 15 min. Stirring was continued at room temperature, then at 80° C. overnight. The mixture was diluted with water and extracted three times with ethyl acetate, dried (anhyd. Na2SO4), filtered and concentrated under vacuum to give a yellow oil. The oil was purified by column chromatography on silica gel using EtOAc-hexanes (0-100% gradient) to give the product (2.8 g) as a yellow solid.

1. customwas continued at room temperature
2. customat 80° C.
3. customovernight
4. extractionextracted three times with ethyl acetate
5. dry with materialdried (anhyd. Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. customto give a yellow oil
9. customThe oil was purified by column chromatography on silica gel