反应详情

0.5 g of 5-tert-butyl-2-methoxy-1-methylsulphanyl-3-nitro-benzene are dissolved in 15 ml of 1,1,1,3,3,3-hexafluoroisopropanol, combined with 1.1 ml of a 9 M solution of hydrogen peroxide in water and stirred for 5 hours at ambient temperature. Then the mixture is cooled to 0° C. and diluted with 10% aqueous sodium thiosulphate solution. The mixture is extracted 3 times with ethyl acetate and the combined organic phases are washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution. After drying with sodium sulphate the solvents are eliminated in vacuo and the residue is chromatographed on silica gel (petroleum ether/ethyl acetate 95:5).

1. temperatureThen the mixture is cooled to 0° C.
2. extractionThe mixture is extracted 3 times with ethyl acetate
3. washthe combined organic phases are washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution
4. dry with materialAfter drying with sodium sulphate the solvents
5. customthe residue is chromatographed on silica gel (petroleum ether/ethyl acetate 95:5)