反应详情

温度

90 °C

A solution of methyl 3-bromo-6-dibromomethyl-2-methoxybenzoate (Intermediate 42A, 19 g) in DMA (300 mL) was added to a stirred solution of sodium benzenesulfinate 17.9 g) and sodium hydrogen carbonate (9.5 g) in water (70 mL) and the mixture was heated at 90° C. for 2 hours. After cooling, the mixture was poured into water and filtered through Celite and the pad was washed with ethyl acetate. The organic layer was separated, washed with water and brine, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and pentane with a gradient of 0-100% to give methyl 6-(benzenesulfonylmethyl)-3-bromo-2-methoxybenzoate (13.8 g).

1. temperatureAfter cooling
2. filtrationfiltered through Celite
3. washthe pad was washed with ethyl acetate
4. customThe organic layer was separated
5. washwashed with water and brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customThe filtrate was evaporated to dryness
9. customthe residue was purified by chromatography on silica
10. washeluting with a mixture of ethyl acetate and pentane with a gradient of 0-100%