反应详情

温度

90 °C

A mixture of ethyl 3-bromo-6-(dibromomethyl)-2-methoxybenzoate (Intermediate 88, 0.25 g), sodium bicarbonate (0.122 g) and sodium 4-chlorobenzenesulphinate (0.29 g) in dimethylacetamide (4 ml) and water (1 ml) was stirred and heated at 90° C. for 5 hours. After cooling, the mixture was diluted with water and loaded onto a water washed C-18 column which was then flushed with water and eluted with DCM and ethyl acetate. The organic eluent was 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 cyclohexane with a gradient of 0-100% to give ethyl 6-(4-chlorobenzenesulphonylmethyl)-3-bromo-2-methoxy-benzoate (0.15 g) as a gum.

1. temperatureAfter cooling
2. customwas then flushed with water
3. washeluted with DCM and ethyl acetate
4. dry with materialThe organic eluent was dried (MgSO4)
5. filtrationfiltered
6. customThe filtrate was evaporated to dryness
7. customthe residue was purified by chromatography on silica
8. washeluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-100%