反应详情

To a stirred mixture of 2-bromo-4-chloroaniline (5 g, 24 mmol) and catalytic DMAP in CH2Cl2 (15 mL) was add acetic anhydride (2.3 mL, 24 mmol) at room temperature. The reaction mixture was stirred overnight then washed with saturated aqueous NaHCO3 solution. The CH2Cl2 layer was dried (MgSO4), filtered, concentrated in vacuo. The crude material was triturated with Hexane/Et2O and the solid filtered and dried in vacuo to give N-(2-bromo-4-chloro-phenyl)-acetamide (5.2 g, 86%). HPLC: Rt=2.26 min. m/z=248 (M+H+).

1. washthen washed with saturated aqueous NaHCO3 solution
2. dry with materialThe CH2Cl2 layer was dried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude material was triturated with Hexane/Et2O
6. filtrationthe solid filtered
7. customdried in vacuo