反应详情

A solution of 3-chloro-4-fluorobenzenethiol (1.0 g), 1-(bromomethyl)-4-fluorobenzene (1.15 g) and potassium carbonate (0.85 g) in DMF (10 ml) was stirred overnight at RT then diluted with water, extracted with ether, and the organics dried (MgSO4) and evaporated under reduced pressure. The resulting oil was dissolved in DCM (10 ml) and MCPBA (1.2 g) added and stirred at RT overnight. The solution was then washed with aqueous sodium metabisulphite and aqueous sodium hydrogen carbonate, dried (MgSO4) and evaporated under reduced pressure to give an oil which was purified by flash column chromatography (eluting 3:2 i-hexane/ether) to give the subtitle compound as a white solid (1.3 g).

1. extractionextracted with ether
2. dry with materialthe organics dried (MgSO4)
3. customevaporated under reduced pressure
4. dissolutionThe resulting oil was dissolved in DCM (10 ml)
5. additionMCPBA (1.2 g) added
6. washThe solution was then washed with aqueous sodium metabisulphite and aqueous sodium hydrogen carbonate
7. dry with materialdried (MgSO4)
8. customevaporated under reduced pressure
9. customto give an oil which
10. customwas purified by flash column chromatography (eluting 3:2 i-hexane/ether)