反应详情

温度

100 °C

To a stirred solution of methyl 3,5-dibromo-4-(bromomethyl)benzoate (INTERMEDIATE 24) (12.53 g, 32.4 mmol, 1 eq) in dioxane (100 mL) and water (100 mL) was added CaCO3 (8.1 g, 81 mmol, 2.5 eq). The mixture was warned to and stirred at 100° C. until reaction was complete by HPLC analysis. The mixture was cooled and the solvent removed under reduced pressure. The residue was diluted with water and extracted 3× with CH2Cl2. The organic extracts were combined, dried over anhydrous Na2SO4, filtered and concentrated giving methyl 3,5-dibromo-4-(hydroxymethyl)benzoate. The material was taken immediately to the next step.

1. temperatureThe mixture was cooled
2. customthe solvent removed under reduced pressure
3. additionThe residue was diluted with water
4. extractionextracted 3× with CH2Cl2
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated