反应详情

To a solution of 10 g of o-cresol and 16.5 g (1.2 equiv) NaI in 250 ml of DMF was added 31 g (1.2 equiv) of chloramine-T hydrate. The dark green solution was stirred at rt for 1.5 h. The mixture, now a heterogeneous light brown, was poured into water, acidified, extracted with ethyl acetate, and the organic phase washed with water and bisulfite solution. The organic phase was dried over MgSO4. Concentration, trituration with hexane, and flash chromatography (silica gel, hexane, hexane/ethyl acetate (5:1)) provided 13.6 g (63%) of the title compound as a white solid.

1. extractionextracted with ethyl acetate
2. washthe organic phase washed with water and bisulfite solution
3. dry with materialThe organic phase was dried over MgSO4
4. concentrationConcentration, trituration with hexane, and flash chromatography (silica gel, hexane, hexane/ethyl acetate (5:1))