反应详情

A solution of 7-bromo-2,3-dihydro-4H-thiochromen-4-one (1 g) in trifluoroacetic acid (12 ml) was treated with triethylsilane (1.48 ml) and the mixture was stirred at reflux for 4 h. Water was added and the mixture extracted with ethyl acetate. The organic solution was washed with brine, dried (Na2SO4) and evaporated. The residue was purified by chromatography on a Biotage cartridge (40 g) eluting with petrol-diethyl ether (10:1) to give the title compound (946 mg). LCMS RT=3.71 min

1. temperatureat reflux for 4 h
2. extractionthe mixture extracted with ethyl acetate
3. washThe organic solution was washed with brine
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customThe residue was purified by chromatography on a Biotage cartridge (40 g)
7. washeluting with petrol-diethyl ether (10:1)