反应详情

To a stirred solution of 2-(2,2,2-trifluoroethoxy)-3-chlorotoluene (2.4 g, 11 mmol) from Step 1 above in CCl4 (40 mL) was added NBS (2.1 g, 11 mmol) and AIBN (1.8 g, 11 mmol). The mixture was refluxed for 8 h. The solvent was removed under reduced pressure and the residue was partitioned between EtOAc and saturated aqueous NaHCO3. The organic phase was dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography using hexanes as eluant. 2-(2,2,2-trifluoroethoxy)-3-chlorobenzyl bromide was obtained as an oil (HPLC retention time=22.3 min (method D)).

1. temperatureThe mixture was refluxed for 8 h
2. customThe solvent was removed under reduced pressure
3. customthe residue was partitioned between EtOAc and saturated aqueous NaHCO3
4. dry with materialThe organic phase was dried (MgSO4)
5. filtrationfiltered
6. customthe solvent was removed under reduced pressure
7. customThe residue was purified by silica gel column chromatography