反应详情

To a solution of 5-methyl-2-(2-trifluoromethyl-biphenyl-4-yl)-benzo[b]thiophene (184 mg, 0.5 mmol) in CHCl3 (2.5 mL) is added SO2Cl2 (44 μL, 1.1 eq.). The mixture is heated to reflux overnight (about 14 hours). All the solvent is removed under reduced pressure. The residue is extracted with CH2Cl2 (50 mL), washed with saturated aqueous NaHCO3, brine, dried over MgSO4, filtered, and concentrated to give an oil. The mixture is purified by column chromatography (EtOAc/Hexane, gradient) to give 112 mg of 3-chloro-5-methyl-2-(2-trifluoromethyl-biphenyl-4-yl)-benzo[b]thiophene in 56% yield.

1. temperatureThe mixture is heated
2. temperatureto reflux overnight (about 14 hours)
3. customAll the solvent is removed under reduced pressure
4. extractionThe residue is extracted with CH2Cl2 (50 mL)
5. washwashed with saturated aqueous NaHCO3, brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customto give an oil
10. customThe mixture is purified by column chromatography (EtOAc/Hexane, gradient)