反应详情

To a suspension of sodium 5-bromo-2-methoxybenzenesulfinate (1.99 g) in DMF (873 ml) was added iodomethane (32 ml). The reaction mixture turned yellow and was stirred at room temperature for 2 hours. The reaction was quenched by the addition of water (ca. 5 ml). The mixture was diluted with EtOAc and extracted with 5% LiCl (3×) and brine (1×). The organic layer was dried (Na2SO4/MgSO4) and filtered. The filtrate was concentrated and purified by silica gel column chromatography to give 1.62 g 4-bromo-1-methoxy-2-(methylsulfonyl)benzene as a white crystalline solid.

1. customThe reaction was quenched by the addition of water (ca. 5 ml)
2. additionThe mixture was diluted with EtOAc
3. extractionextracted with 5% LiCl (3×) and brine (1×)
4. dry with materialThe organic layer was dried (Na2SO4/MgSO4)
5. filtrationfiltered
6. concentrationThe filtrate was concentrated
7. custompurified by silica gel column chromatography