反应详情

A solution of 2,4-dibromobenzoic acid (52.0 g, 176 mmol, 1.00 equiv, 95%) and sulfuric acid (20 mL) in methanol (400 mL) was stirred at 90° C. overnight. After cooling to room temperature, the mixture was concentrated under reduced pressure. The residue was diluted with 500 mL of ethyl acetate and washed with 3×100 mL of H2O followed by 1×100 mL of NaHCO3 (aq., sat. Note: gas evolution occurs). The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo. This resulted in 45.0 g (78%) of methyl 2,4-dibromobenzoate as a yellow oil.

1. concentrationthe mixture was concentrated under reduced pressure
2. additionThe residue was diluted with 500 mL of ethyl acetate
3. washwashed with 3×100 mL of H2O
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. customThis resulted in 45.0 g (78%) of methyl 2,4-dibromobenzoate as a yellow oil