反应详情

Methanol (40 mL) was added to a 250 mL round bottom flask followed by 60 mL of a solution saturated with anhydrous hydrochloric acid. 3-bromo-5-iodobenzoic acid (Aldrich)(5.02 g, 0.015 mole) was then added and the reaction mixture was stirred at room temperature for 6 hours. The reaction mixture was poured into chilled saturated NaHCO3 solution (700 mL). The mixture was extracted 3× with methylene chloride (100 mL). The organic layers were combined, dried over MgSO4 and concentrated under vacuum to yield methyl-5-bromo-3-iodobenzoate (5.08 g) as a pink solid. MP=55-57° C. MS and NMR were consistent with the desired structure.

1. additionThe reaction mixture was poured
2. extractionThe mixture was extracted 3× with methylene chloride (100 mL)
3. dry with materialdried over MgSO4
4. concentrationconcentrated under vacuum