反应详情

3,4-difluoroaniline (3.5 g), acetonitrile (60 ml), diphenyldisulfide (6 g) and isoamyl nitrite (8 ml) were charged to a flask and heated at 60° C. for 2 h then evaporated under reduced pressure. The residue was purified by flash column chromatography (eluent isohexane) to give the subtitle compound. The product (3,4-difluorophenyl phenyl sulfide) was dissolved in acetonitrile (60 ml). Water (10 ml) and oxone (20 g) were added and stirred for 72 h at RT. The reaction mixture was partitioned between ether/water, the organics were separated, washed with water, then dried (MgSO4) and evaporated under reduced pressure. The residue was purified by flash column chromatography (eluent 5-10% ethyl acetate/isohexane) to give the subtitle compound (2.14 g).

1. customThe reaction mixture was partitioned between ether/water
2. customthe organics were separated
3. washwashed with water
4. dry with materialdried (MgSO4)
5. customevaporated under reduced pressure
6. customThe residue was purified by flash column chromatography (eluent 5-10% ethyl acetate/isohexane)