反应详情

Dissolve 2-trifluoromethyl-benzenethiol (10 g, 56 mmol), potassium carbonate (25 g, 180 mmol), iodomethane (11 mL, 177 mmol) in DMF (100 mL). Stir for 12 hours. Filter the suspension through a pad of silica gel and elute with ethyl acetate (500 mL). Evaporate half of the solvent and wash the remaining solution with 10% aqueous LiCl (100 mL). Dry with MgSO4 and evaporate solvent. Chromatograph the residue on a SiO2 column eluting with hexane to give 9.5 g of 1-methylsulfanyl-2-trifluoromethyl-benzene (88%).

1. filtrationFilter the suspension through a pad of silica gel
2. washelute with ethyl acetate (500 mL)
3. customEvaporate half of the solvent
4. washwash the remaining solution with 10% aqueous LiCl (100 mL)
5. dry with materialDry with MgSO4
6. customevaporate solvent
7. washChromatograph the residue on a SiO2 column eluting with hexane