反应详情

428 mg (2.64 mmol) of iron(III) chloride was added to a mixture of 16.86 g (92.02 mmol) of 1-ethylsulfanyl-4-nitrobenzene in 75 ml acetonitrile and it was stirred for 10 minutes at room temperature. Then 22.44 g (98.44 mmol) of periodic acid was added in portions, so that the temperature did not exceed 30° C. The mixture was stirred for 50 minutes and was then added, with stirring, to a mixture of 170 ml DCM, 500 ml ice water and 100 g sodium thiosulfate pentahydrate. It was extracted with DCM (2×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. The residue obtained was recrystallized from ethyl acetate/hexane. 12.49 g (62.69 mmol; yield: 68%) of the product was obtained.

1. customdid not exceed 30° C
2. stirringThe mixture was stirred for 50 minutes
3. additionwas then added
4. extractionIt was extracted with DCM (2×)
5. dry with materialThe combined organic phases were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated by evaporation
8. customThe residue obtained
9. customwas recrystallized from ethyl acetate/hexane
10. custom12.49 g (62.69 mmol; yield: 68%) of the product was obtained