反应详情

To a solution of 3-trifluoroacetyl-1,2,4,5-tetrahydro-3-benzazepine-7-sulfonyl fluoride (D1) (5.3 g, 17 mmol) in trifluoromethanesulfonic acid (30 ml) at 0° C. was added portionwise N-iodosuccinimide (5.9 g, 25 mmol). The resulting solution was stirred for 1 h without cooling then poured into saturated aqueous sodium hydrogencarbonate (200 ml) containing sodium sulfite (1 g), extracted with ethyl acetate (100 ml), and the resulting organic layer washed with brine (100 ml), dried (MgSO4), and evaporated. Chromatography on silica, eluting with 3:1 hexane:ethyl acetate gave the subtitle compound as a white solid (5.2 g).

1. temperaturewithout cooling
2. extractionextracted with ethyl acetate (100 ml)
3. washthe resulting organic layer washed with brine (100 ml)
4. dry with materialdried (MgSO4)
5. customevaporated
6. washChromatography on silica, eluting with 3:1 hexane