反应详情

温度

75 °C

A solution of N-trifluoroacetyl-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (2.5 g, 8.5 mmol) in 1,2-dichloroethane (15 mL) was treated with Selectfluor (3.9 g, 11 mmol), trifluoromethanesulfonic acid (8 mL, 90 mmol) and stirred 60 hours at 75° C. The product mixture was poured into water (200 mL), extracted with EtOAc (200 mL), the organic phase washed with saturated aqueous NaHCO3 (2×100 mL), brine (100 mL), dried with Na2SO4 and concentrated. The crude product was purified by flash chromatography (6% EtOAc in hexane, silica) resulting in 0.6 g of a white solid. MS calculated for C13H12ClF4NO+H: 310, observed: 310.

1. extractionextracted with EtOAc (200 mL)
2. washthe organic phase washed with saturated aqueous NaHCO3 (2×100 mL), brine (100 mL)
3. dry with materialdried with Na2SO4
4. concentrationconcentrated
5. customThe crude product was purified by flash chromatography (6% EtOAc in hexane, silica)